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Journal articles on the topic 'SPME'

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Author: Grafiati
Published: 4 June 2021
Last updated: 25 May 2024

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1

Musiman, Musiman, and Muhammad Kristiawan. "Evaluasi Sistem Penjaminan Mutu Program Studi S1 Pendidikan Sekolah Dasar STKIP Muhammadiyah Oku Timur." Jurnal Basicedu 5, no. 6 (October 14, 2021): 5070–77. http://dx.doi.org/10.31004/basicedu.v5i6.1591.

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Pada sistem Penjaminan Mutu Internal (SPMI) belum menjadi prioritas oleh sebagian besar perguruan tinggi jika dibandingkan dengan Sistem Penjaminan Mutu Eksternal (SPME). Amanat UU Nomor 12 Tahun 2012 tentang Pendidikan Tinggi menyebutkan bahwa SPMI dan SPME merupakan bagian dari suatu sistem. Diduga SPMI oleh beberapa Perguruan Tinggi tidak memberikan dampak yang signifikan seperti SPME dimana Perguruan Tinggi akan mendapatkan hasil Akreditasi. Penelitian ini dilakukan pada periode Agustus sampai dengan Desember 2019. Tujuan penelitian ini adalah dalam rangka mengevaluasi Program SPMI yang dikembangkan oleh Program Pendidikan Anak Usia Dini Terakreditasi (PGSD) C. Metode penilaian dilakukan dengan menggunakan pendekatan sistem yang meliputi aspek konteks, masukan, proses, dan keluaran, dengan mengacu pada studi literatur hasil penelitian yang relevan. Hasil pelaksanaan SPMI di prodi PAUD sudah berjalan dengan baik, jika dibandingkan dengan PPEPP semua aspek tahapan pelaksanaannya. Rekomendasi evaluasi SPMI dalam penelitian ini ditujukan kepada tiga pemangku kepentingan, yaitu Direktorat Penjaminan Mutu, Badan Penjaminan Mutu tingkat Universitas, dan Ketua Program Studi
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2

Ragil, Yoga Aditia, Sri Martini Meilani, and Zarina Akbar. "Evaluasi Sistem Penjaminan Mutu Internal Program Studi S1 Pendidikan Guru Pendidikan Anak Usia Dini." Jurnal Obsesi : Jurnal Pendidikan Anak Usia Dini 4, no. 2 (January 11, 2020): 567. http://dx.doi.org/10.31004/obsesi.v4i2.420.

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Sistem Penjaminan Mutu Internal (SPMI) belum menjadi prioritas oleh sebagian besar Perguruan Tinggi bila dibandingkan Sistem Penjaminan Mutu Eksternal (SPME). Amanah Undang-Undang Nomor 12 Tahun 2012 tentang Pendidikan Tinggi menyatakan SPMI dan SPME merupakan bagian dari suatu sistem. Diduga SPMI oleh sebagian Perguruan Tinggi tidak memberikan dampak yang signifikan seperti SPME dimana Perguruan Tinggi akan mendapatkan hasil Akreditasi. Penelitian ini dilakukan pada periode Agustus sampai dengan Desember 2019. Tujuan penelitian ini dalam rangka mengevaluasi Program SPMI yang dikembangkan oleh Program Studi Pendidikan Anak Usia Dini (PAUD) yang terakreditasi C. Metode pengkajian dilakukan menggunakan pendekatan sistem meliputi aspek konteks, input, proses, dan output, dengan mengacu kepada studi literatur pada hasil-hasil penelitian yang relevan. Hasil pelaksanaan SPMI pada prodi PAUD sudah berjalan dengan baik, bila dibandingkan dengan PPEPP seluruh aspek sudah ditahap pelaksanaan. Rekomendasi evaluasi SPMI pada penelitian ini ditujukan kepada tiga pemangku kepentingan yaitu Direktorat Penjaminan Mutu, Lembaga Penjaminan Mutu tingkat Universitas, dan pimpinan Program Studi.
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3

HORÁK, Tomáš, Jiří ČULÍK, Marie JURKOVÁ, Pavel ČEJKA, and Vladimír KELLNER. "Application of SPE and SPME in Analysis of Beer." Kvasny Prumysl 52, no. 3 (March 1, 2006): 78–82. http://dx.doi.org/10.18832/kp2006006.

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4

., Sugiyo. "PENTINGNYA PENYELARASAN SPMI DAN SPME DALAM IMPLEMENTASI SISTEM PENJAMINAN MUTU INTERNAL PERGURUAN TINGGI." JURNAL MATEMAR: MANAJEMEN DAN TEKNOLOGI MARITIM 2, no. 1 (August 16, 2023): 1–10. http://dx.doi.org/10.59225/matemar.v2i1.67.

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Sistem Penjaminan Mutu Pendidikan Tinggi (SPM PT) merupakan standar pendidikan tinggi yang terdiri dari Sistem Penjaminan Mutu Internal (SPMI) yang memiliki siklus tentang Penetapan Standar Dikti, Pelaksanaan Standar Dikti, Evaluasi (pelaksanaan) standar Dikti, Pengendalian (pelaksanaan) standar Dikti dan Peningkatan (pelaksanaan) standar Dikti yang disebut dengan PPEPP. Sedangkan Sistem Penjaminan Mutu Eksternal (SPME) yang memiliki siklus Evaluasi Data dan Informasi, Penetapan Status Akreditasi dan Peringkat Terakreditasi, Pemantauan dan Evaluasi Status Akreditasi dan Peringkat Akreditasi yang disebut dengan EPP. SPMI diimplementasikan pada semua bidang kegiatan perguruan tinggi yaitu Bidang Akademik, yang meliputi bidang pendidikan, bidang penelitian, Bidang pengabdian kepada masyarakat; dan Bidang Non-Akademik yang meliputi Sumber Daya Manusia (SDM), Keuangan, dan sarana dan prasarana. Perencanaan, pelaksanaan, evaluasi, pengendalian, dan pengembangan SPMI dan SPME didasarkan pada Standar Dikti memiliki siklus PPEPP dan metode Evaluasi dilakukan melalui Audit Mutu Internal (AMI), dengan demikian menghasilkan luaran / Output bahwa luaran penerapan SPMI oleh PT digunakan oleh BAN PT atau LAM PT untuk penetapan Status dan peringkat terakreditasi PT dan Program Studi.
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5

Trofin, Alina Elena, Lucia Carmen Trincă, Elena Ungureanu, and Adina Mirela Ariton. "CUPRAC Voltammetric Determination of Antioxidant Capacity in Tea Samples by Using Screen-Printed Microelectrodes." Journal of Analytical Methods in Chemistry 2019 (May 14, 2019): 1–10. http://dx.doi.org/10.1155/2019/8012758.

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Measurement of antioxidant capacity represents an analytical major challenge in terms of accuracy, efficiency, rapid response, or low cost of detection methods. Quantification of antioxidant capacity of food samples using disposable screen‐printed microelectrodes (SPMEs) was based on cyclic voltammetry versus open-circuit potential (CV vs OCP) and differential pulse voltammetry (DPV) as compared with spectrophotometric measurement of the CUPRAC reaction with 6-hydroxy-2,5,7,8-tetramethylchroman-2-carboxylic acid (trolox). The SPMEs are organic‐resistant electrodes and thus compatible with food samples and organic solvents used to dissolve trolox. A micropipette was used to release a drop of 50 μL sample on the spotted surface of the SPME sensor/working electrode that was time programmed to function according to the working protocol. The SPME response was linearly correlated with trolox content. This preliminary demonstration was focused on the analysis of tea infusions, due to the simplicity and reproducibility of the samples’ preparations involved. Analytical results of the antioxidant capacity (expressed as mol·L−1 trolox equivalents) of the tea samples showed a good agreement in the case of spectrophotometry and differential pulse voltammetry (R2 > 0.998). DPV with SPME based on CUPRAC reactions was proven to be a promising approach for the characterization of antioxidant capacity of tea samples with rapid response, cost-effectiveness, and simplicity of operation.
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6

Manousi, Natalia, Erwin Rosenberg, and George A. Zachariadis. "Solid-Phase Microextraction Arrow for the Sampling of Volatile Organic Compounds in Milk Samples." Separations 7, no. 4 (December 18, 2020): 75. http://dx.doi.org/10.3390/separations7040075.

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A novel sample preparation method based on the use of the Arrow solid-phase microextraction device was used to extract and preconcentrate volatile organic compounds (VOCs) from milk samples prior to their determination by gas chromatography–mass spectrometry (GC-MS). The experimental parameters of the solid-phase microextraction (SPME) Arrow method were evaluated in terms of fiber type, sample volume, extraction temperature, extraction time, stirring rate and salt addition. Under the optimum extraction conditions, the SPME Arrow was compared with conventional SPME fibers to evaluate the effectiveness of the SPME Arrow method. Evaluation of the conventional SPME procedure was also performed under optimized conditions, for appropriate method comparison. Due to the larger sorption phase volume of SPME Arrow, a higher sensitivity and reproducibility were observed for the determined chromatographic peaks in comparison with conventional SPME fibers. The use of Carbon wide range (WR) SPME Arrow/polydimethylsiloxane (CAR/PDMS) SPME Arrow fibers leads to a compound-dependent improvement of a factor of 4–5x over the classical SPME setup. Moreover, the relative standard deviation (RSD) of the total volatiles for a conventional SPME procedure was 12.5%, while for SPME Arrow it was 6.2%. Finally, the novel method was successfully employed for the analysis of commercially available milk samples. The findings of this study indicate that SPME Arrow can be effectively used for the determination of volatile organic compounds in complex food matrixes.
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7

Guidotti, Maurizio. "Determination of Se4+ in Drinkable Water by Solid-Phase Microextraction and Gas Chromatography/Mass Spectrometry." Journal of AOAC INTERNATIONAL 83, no. 5 (September 1, 2000): 1082–86. http://dx.doi.org/10.1093/jaoac/83.5.1082.

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Abstract A method was developed for the selective determination of Se4+ in drinkable water by solid-phase microextraction (SPME) and gas chromatography/mass spectrometry (GC/MS). Se4+ was selectively derivatized to ethane, 1,1′-selenobis by reaction with sodium tetraethylborate, extracted by the SPME fiber, and determined by GC/MS. Both headspace (HS)–SPME and direct SPME were studied. The method requires only a few milliliters of sample and 20 min for completion. At 2.0 μg/L concentration, the relative standard deviation was 10.1% for HS–SPME and 9.1% for direct SPME. For HS–SPME, the theoretical detection limit was 81 ng/L and 166 ng/L for direct SPME. The recovery rate was 95%. The method was used to determine Se4+ in 10 tap water samples.
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8

Alsayadi, Yunes M. M. A., and Saahil Arora. "A review: Total vaporization solid-phase microextraction procedure in different matrixes." Analytical Methods in Environmental Chemistry Journal 5, no. 03 (September 29, 2022): 80–102. http://dx.doi.org/10.24200/amecj.v5.i03.190.

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Total vaporization solid-phase microextraction (TV-SPME) is a type of extraction technique in which a specific solvent dissolves the analyte. Then a tiny amount of solvent is taken to the vial of SPME. Then, the solvent vaporizes in the SPME vial, and sampling is carried out on the headspace of the SPME fiber. As a result, the partitioning phase of the analyte between the headspace and liquid sample is omitted. The equilibrium phase remains the analyte partitioning between the headspace and SPME. TV-SPME was introduced in 2014 by Goodpaster to increase the recovery compared to the liquid injection method. This review discusses different aspects of TV-SPME, including its impact on sampling techniques, theoretical part, sampling procedure, and method optimization. Special attention was paid to its applications. A comprehensive literature study was conducted in the relevant databases to summarize the research work that has been done on this technique. In TV-SPME, the liquid samples completely vaporized and had a less matrix effect and better adsorption. This method needs no sample preparation, consumes less supply, and can be done automatically. Also, TV-SPME enables a cost-effective and efficient extraction for different matrixes. This review summarizes aspects related to TV-SPME.
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9

Mugo, Samuel M., Scott V. Robertson, and Marika Wood. "A Hybrid Stainless-Steel SPME Microneedle Electrode Sensor for Dual Electrochemical and GC-MS Analysis." Sensors 23, no. 4 (February 19, 2023): 2317. http://dx.doi.org/10.3390/s23042317.

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A mechanically robust in-tube stainless steel microneedle solid phase microextraction (SPME) platform for dual electrochemical and chromatographic detection has been demonstrated. The SPME microneedle was fabricated by layer-by-layer (LbL) in-tube coating, consisting of carbon nanotube (CNT)/cellulose nanocrystal (CNC) film layered with an electrically conductive polyaniline (PANI) hydrogel layer (PANI@CNT/CNC SPME microneedle (MN)). The PANI@CNT/CNC SPME MN showed effective analysis of caffeine by GC-MS with an LOD of 26 mg/L and excellent precision across the dynamic range. Additionally, the PANI@CNT/CNC SPME MN demonstrated a 67% increase in sensitivity compared to a commercial SPME fiber, while being highly robust for repeated use without loss in performance. For electrochemical detection, the PANI@CNT/CNC SPME MN showed excellent performance for the detection of 3-caffeoylquinic acid (3-CQA). The dynamic range and limits of detection (LOD) for 3-CQA analysis were 75–448 mg/L and 11 mg/L, respectively. The PANI@CNT/CNC SPME MN was demonstrated to accurately determine the caffeine content and 3-CQA in tea samples and dark roast coffee, respectively. The PANI@CNT/CNC SPME MN was used for semiquantitative antioxidant determination and composition analysis in kiwi fruit using electrochemistry and SPME-coupled GC-MS, respectively.
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10

(Mel) Suffet, I. H., A. Bruchet, and C. C. Young. "Development of a closed loop stripping analysis using solid-phase microextraction to analyze geosmin and MIB in drinking water." Water Supply 6, no. 3 (July 1, 2006): 167–74. http://dx.doi.org/10.2166/ws.2006.800.

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A novel analytical method, solid phase microextraction (SPME) coupled with closed loop stripping analysis (CLSA), was introduced for the analysis of MIB and geosmin at nanogram per liter concentration levels. The optimum CLSA/SPME analysis conditions of 65 °C, 60-minute extraction time, and 0.5 M sodium sulfate were determined from a statistical design. The individual Kfw of MIB and geosmin from CLSA/SPME method was 4.21 and 4.85, and resulted an order of magnitude greater than the Kfw obtained from direct SPME method. A detection limit of 10 ng/L of MIB and geosmin was achieved by GC-MS with CLSA/SPME with a polyacrylate phase. Overall, CLSA/SPME provides a fast, solvent-free, and less labor intensive method compared to the standard CLSA. The CLSA/SPME method is a valuable alternative method for the analysis of taste-and-odor causing compounds in drinking water.
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11

Tajik, Leila, Abdulrahman Bahrami, Alireza Ghiasvand, and Farshid Ghorbani Shahna. "Determination of benzene, toluene, ethylbenzene and xylene in field and laboratory by means of cold fiber SPME equipped with thermoelectric cooler and GC/FID method." Polish Journal of Chemical Technology 19, no. 3 (September 1, 2017): 9–15. http://dx.doi.org/10.1515/pjct-2017-0041.

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Abstract A simple and effective cooling device based on a thermoelectric cooler was applied to cool the SPME fiber. The device was used for quantitative extraction of aromatic hydrocarbons in the air. Several factors such as coating temperature, extraction temperature and relative humidity in the laboratory setting were optimized. Comparison of the results between the cold fiber SPME (CF-SPME) and NIOSH 1501 method on standard test atmosphere indicated a satisfactory agreement. The CF-SPME and SPME method were also compared. The results revealed that CF-SPME has the most appropriate outcome for the extraction of aromatic hydrocarbons from the ambient air. The cold fiber SPME technique showed good results for several validation parameters. Under the optimized conditions, the limits of detection (LOD) and the limits of quantification (LOQ) ranged from 0.00019 to 0.00033 and 0.0006 to 0.001 ng ml−1, respectively. The intra-day relative standard deviation (RSD) showed ranging from 4.8 to 10.5%.
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12

Bojko, Barbara, Erasmus Cudjoe, German A. Gómez-Ríos, Krzysztof Gorynski, Ruifen Jiang, Nathaly Reyes-Garcés, Sanja Risticevic, et al. "SPME – Quo vadis?" Analytica Chimica Acta 750 (October 2012): 132–51. http://dx.doi.org/10.1016/j.aca.2012.06.052.

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13

Dugheri, Stefano, Giovanni Cappelli, Niccolò Fanfani, Jacopo Ceccarelli, Giorgio Marrubini, Donato Squillaci, Veronica Traversini, Riccardo Gori, Nicola Mucci, and Giulio Arcangeli. "A New Perspective on SPME and SPME Arrow: Formaldehyde Determination by On-Sample Derivatization Coupled with Multiple and Cooling-Assisted Extractions." Molecules 28, no. 14 (July 16, 2023): 5441. http://dx.doi.org/10.3390/molecules28145441.

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Formaldehyde (FA) is a toxic compound and a human carcinogen. Regulating FA-releasing substances in commercial goods is a growing and interesting topic: worldwide production sectors, like food industries, textiles, wood manufacture, and cosmetics, are involved. Thus, there is a need for sensitive, economical, and specific FA monitoring tools. Solid-phase microextraction (SPME), with O-(2,3,4,5,6-pentafluorobenzyl)-hydroxylamine (PFBHA) on-sample derivatization and gas chromatography, is proposed for FA monitoring of real-life samples. This study reports the use of polydimethylsiloxane (PDMS) as a sorbent phase combined with innovative commercial methods, such as multiple SPME (MSPME) and cooling-assisted SPME, for FA determination. Critical steps, such as extraction and sampling, were evaluated in method development. The derivatization was performed at 60 °C for 30 min, followed by 15 min sampling at 10 °C, in three cycles (SPME Arrow) or six cycles (SPME). The sensitivity was satisfactory for the method’s purposes (LOD-LOQ at 11-36 ng L−1, and 8-26 ng L−1, for SPME and SPME Arrow, respectively). The method’s linearity ranges from the lower LOQ at trace level (ng L−1) to the upper LOQ at 40 mg L−1. The precision range was 5.7–10.2% and 4.8–9.6% and the accuracy was 97.4% and 96.3% for SPME and SPME Arrow, respectively. The cooling MSPME set-up applied to real commercial goods provided results of quality comparable to previously published data.
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Shen, Shun, Yunfei Sha, Chunhui Deng, Daxi Fu, Jiakuan Chen, and Xiangmin Zhang. "Comparison of Solid-Phase Microextraction, Supercritical Fluid Extraction, Steam Distillation, and Solvent Extraction Techniques for Analysis of Volatile Consituents in Fructus Amomi." Journal of AOAC INTERNATIONAL 88, no. 2 (March 1, 2005): 418–23. http://dx.doi.org/10.1093/jaoac/88.2.418.

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Abstract Four sampling techniques, solid-phase microextraction (SPME), supercritical fluid extraction (SFE), steam distillation (SD), and solvent extraction (SE), were compared for the analysis of volatile constituents from a traditional Chinese medicine (TCM) of the dried ripe fruit of Fructus Amomi (Sha Ren). A total of 38 compounds were identified by gas chromatography/mass spectrometry. Different SFE and SPME parameters (modifier content, extraction pressure, and temperature for SFE and fibers, extraction temperature, and time for SPME) were studied. The results by SFE and SPME were compared with those obtained by conventional SD and SE methods. The results showed that SFE and SPME are better sample preparation techniques than SD and SE. Due to SFE's requirement for expensive specialized instrumentation, the simplicity, low cost, and speed of SPME make it a more appropriate technique for extraction of volatile constituents in TCMs.
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15

Schulz, Eray, Mark Woollam, Paul Grocki, Michael D. Davis, and Mangilal Agarwal. "Methods to Detect Volatile Organic Compounds for Breath Biopsy Using Solid-Phase Microextraction and Gas Chromatography–Mass Spectrometry." Molecules 28, no. 11 (June 3, 2023): 4533. http://dx.doi.org/10.3390/molecules28114533.

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Volatile organic compounds (VOCs) are byproducts from metabolic pathways that can be detected in exhaled breath and have been reported as biomarkers for different diseases. The gold standard for analysis is gas chromatography–mass spectrometry (GC–MS), which can be coupled with various sampling methods. The current study aims to develop and compare different methods for sampling and preconcentrating VOCs using solid-phase microextraction (SPME). An in-house sampling method, direct-breath SPME (DB–SPME), was developed to directly extract VOCs from breath using a SPME fiber. The method was optimized by exploring different SPME types, the overall exhalation volume, and breath fractionation. DB–SPME was quantitatively compared to two alternative methods involving the collection of breath in a Tedlar bag. In one method, VOCs were directly extracted from the Tedlar bag (Tedlar–SPME) and in the other, the VOCs were cryothermally transferred from the Tedlar bag to a headspace vial (cryotransfer). The methods were verified and quantitatively compared using breath samples (n = 15 for each method respectively) analyzed by GC–MS quadrupole time-of-flight (QTOF) for compounds including but not limited to acetone, isoprene, toluene, limonene, and pinene. The cryotransfer method was the most sensitive, demonstrating the strongest signal for the majority of the VOCs detected in the exhaled breath samples. However, VOCs with low molecular weights, including acetone and isoprene, were detected with the highest sensitivity using the Tedlar–SPME. On the other hand, the DB–SPME was less sensitive, although it was rapid and had the lowest background GC–MS signal. Overall, the three breath-sampling methods can detect a wide variety of VOCs in breath. The cryotransfer method may be optimal when collecting a large number of samples using Tedlar bags, as it allows the long-term storage of VOCs at low temperatures (−80 °C), while Tedlar–SPME may be more effective when targeting relatively small VOCs. The DB-SPME method may be the most efficient when more immediate analyses and results are required.
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Farooq, Muhammad Shoaib, Uzma Omer, and Rabia Tahseen. "Software Project Management Education: A Systematic Review." VFAST Transactions on Software Engineering 9, no. 3 (September 30, 2021): 102–19. http://dx.doi.org/10.21015/vtse.v9i3.702.

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Software project management (SPM) is a significant field, related to the discipline of software engineering, which has attracted a huge number of researchers and practitioners in recent years. The role of software project management education (SPME) is essential to instill appropriate competencies in SPM students so that they could be able to deliver effectively in the software industry as SPM professionals. As the demand of SPM professionals is continuously increasing, the responsibilities of academia have also been increased to ensure and provide the solid basis and quality education to SPM. In this context, a number of methods and tools have been deliberated to examine SPME from various dimensions. The usefulness of these methods and tools need to be synthesized and evaluated to investigate the areas that could be used to improve the various aspects of SPME. The main objective of this research is to evaluate the techniques that have been applied to teach SPME and identify the future directions that could lead to make improvements in SPME. This article presents a review of eighty-nine research papers of SPME that have been classified and synthesized according to different aspects of SPME. These aspects include type and approach of conducted research, empirical type, SPM knowledge areas, and curricula. The principal findings emerged after analyzing the results of reviewing the SPME research have been discussed in detail. Lastly, a list of advice to SPM instructors, based on the prominent and effective practices of SPME, has also been presented in this study.
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CHEN, HAOXIN, CHUNRONG WANG, ZHIYUN ZHANG, and LILI HE. "Combining Headspace Solid-Phase Microextraction and Surface-Enhanced Raman Spectroscopy To Detect the Pesticide Fonofos in Apple Juice." Journal of Food Protection 81, no. 7 (June 13, 2018): 1087–92. http://dx.doi.org/10.4315/0362-028x.jfp-17-505.

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ABSTRACT We developed an innovative approach that couples headspace solid-phase microextraction (SPME) with surface-enhanced Raman spectroscopy (SERS) to detect a volatile pesticide (i.e., fonofos) in a liquid complex matrix (i.e., apple juice). A gold nanoparticles–coated fiber was fabricated by reducing gold(III) on a chemically etched stainless steel wire to extract pesticide, using SPME. The fabricated fibers were then tested by a headspace-SPME method and a dip-SPME method, followed by SERS detection of fonofos in water and apple juice samples. Using the headspace-SPME method, we can detect as low as 5 ppb of fonofos in water and apple juice, compared with the dip-SPME method, which cannot detect lower than 10 ppb in water and 50 ppb in apple juice. This study demonstrated the potential capability of the headspace-SPME-SERS method for rapid (within 30 min) and sensitive detection of volatile and vaporizable compounds in complex matrices. The developed method could be a potential alternative approach to the gas chromatography method. Future work is needed to optimize the fiber by minimizing signal variation, and it should be tested in a variety of targeted compounds and matrices.
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Naccarato and Tagarelli. "Recent Applications and Newly Developed Strategies of Solid-Phase Microextraction in Contaminant Analysis: Through the Environment to Humans." Separations 6, no. 4 (November 6, 2019): 54. http://dx.doi.org/10.3390/separations6040054.

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The present review aims to describe the recent and most impactful applications in pollutant analysis using solid-phase microextraction (SPME) technology in environmental, food, and bio-clinical analysis. The covered papers were published in the last 5 years (2014–2019) thus providing the reader with information about the current state-of-the-art and the future potential directions of the research in pollutant monitoring using SPME. To this end, we revised the studies focused on the investigation of persistent organic pollutants (POPs), pesticides, and emerging pollutants (EPs) including personal care products (PPCPs), in different environmental, food, and bio-clinical matrices. We especially emphasized the role that SPME is having in contaminant surveys following the path that goes from the environment to humans passing through the food web. Besides, this review covers the last technological developments encompassing the use of novel extraction coatings (e.g., metal-organic frameworks, covalent organic frameworks, PDMS-overcoated fiber), geometries (e.g., Arrow-SPME, multiple monolithic fiber-SPME), approaches (e.g., vacuum and cold fiber SPME), and on-site devices. The applications of SPME hyphenated with ambient mass spectrometry have also been described.
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Emmons, Ronald V., Ramin Tajali, and Emanuela Gionfriddo. "Development, Optimization and Applications of Thin Film Solid Phase Microextraction (TF-SPME) Devices for Thermal Desorption: A Comprehensive Review." Separations 6, no. 3 (August 5, 2019): 39. http://dx.doi.org/10.3390/separations6030039.

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Through the development of solid phase microextraction (SPME) technologies, thin film solid phase microextraction (TF-SPME) has been repeatedly validated as a novel sampling device well suited for various applications. These applications, encompassing a wide range of sampling methods such as onsite, in vivo and routine analysis, benefit greatly from the convenience and sensitivity TF-SPME offers. TF-SPME, having both an increased extraction phase volume and surface area to volume ratio compared to conventional microextraction techniques, allows high extraction rates and enhanced capacity, making it a convenient and ideal sampling tool for ultra-trace level analysis. This review provides a comprehensive discussion on the development of TF-SPME and the applications it has provided thus far. Emphasis is given on its application to thermal desorption, with method development and optimization for this desorption method discussed in detail. Moreover, a detailed outlook on the current progress of TF-SPME development and its future is also discussed with emphasis on its applications to environmental, food and fragrance analysis.
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Vojtěch, Antoš, Hrabák Pavel, Komárek Michal, and Stuchlík Martin. "Polyetherimide Nanofibres as Sorbents for Organochlorinated Pesticides Determination." Journal of Nanomaterials 2016 (2016): 1–7. http://dx.doi.org/10.1155/2016/1390345.

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Electrospun polyetherimide (PEI) nanofibres were fixed on a steel wire solid phase microextraction (SPME) assembly. The basic properties of the prepared nanofibres were determined by thermogravimetry, differential scanning calorimetry, adsorption, and SEM. The analytical performance of prepared PEI SPME fibres was compared with three commercially available SPME fibres, 7 μm PDMS, 100 μm PDMS, and DVB/Carboxene/PDMS. As model water pollutants, persistent organochlorinated pesticides hexachlorocyclohexanes (HCH) and chlorobenzene (ClB) were chosen as model water pollutants. The fibres were compared in the headspace- (HS-) SPME mode of GC-MS/MS instrumentation. The comparison omitted other method parameters and focused exclusively on the extraction time variability. Lab-made PEI SPME fibres showed significantly better response for the target compounds than the other tested fibres from industrial production. Based on the results, the extraction time could be shortened from 50 to 10 min, if PEI SPME fibres were used as a modification of existing analytical protocol.
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Joni Rokhmat, Wildan, Taslim Sjah, Ulpah, and Lulu Il Muntaz. "Peninjauan Dokumen Mutu Pascasarjana Unram untuk Menunjang Penguatan SPMI dan SPME." Jurnal Pengabdian Magister Pendidikan IPA 5, no. 1 (January 17, 2022): 13–17. http://dx.doi.org/10.29303/jpmpi.v5i1.1219.

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Kualitas dokumen mutu merupakan unsur vital dalam penguatan sistem penjaminan mutu internal (SPMI) maupun eksternal (SPME). Tujuan pengabdian ini melakukan peninjauan dokumen mutu Pascasarjana Universitas Mataram meliputi dokumen kebijakan, manual, standar, dan formulism utu. Metode pelaksanaan mengadakan workshop pembahasan dokumen mutu dengan melibatkan pemangku kepentingan yang terdiri dari unsur pimpinan Pascasarjana Unram, beserta staf, program sudi di lingkungan Pascasarjana, Lembaga Penjaminan Mutu dan Pengembangan Pendidikan (LPMPP), serta berbagai lembaga eksternal Unram yang memiliki hubungan kerjasama dalam pengembangan pendidikan. Hasilnya menunjukkan bahwa dokumen mutu yang ada sekarang dengan penetapan tahun 2018 harus dilakukan perbaikan mencakup beberapa hal berikut: 1) perlu menambahkan standar pelampauan di luar delapan standar yang ditetapkan Dikti, 2) perlu menambahkan standar penyelenggarakan MBKM, serta 3) merevisi beberapa konten yang sudah ada seiring dengan dinamika pendidikan yang terus berkembang. Direkomendasikan agar segera dilakukan revisi dokumen mutu yang ada dengan memperhatikan berbagai masukan dari seluruh peserta workshop.
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22

Chen, Mengfei, Hangzhen Lan, Daodong Pan, and Tao Zhang. "Hydrophobic Mesoporous Silica-Coated Solid-Phase Microextraction Arrow System for the Determination of Six Biogenic Amines in Pork and Fish." Foods 12, no. 3 (January 28, 2023): 578. http://dx.doi.org/10.3390/foods12030578.

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In this study, a functionalized mesoporous silica-coated solid-phase microextraction (SPME) Arrow system was developed for the enrichment of six biogenic amines (BAs) from pork and fish samples before gas chromatographic separation with a mass spectrometer as a detector. MCM-41 was utilized as the substrate material and thereby functionalized by titanate and sodium dodecyl sulfate to adjust its surface acidity and hydrophobicity, respectively. The functionalized MCM-41 (named as MCM-T-H) was coated on a bare SPME Arrow using the dipping method and polyacrylonitrile was used as the adhesive. The extraction capacity and selectivity of the MCM-T-H-SPME Arrow for six kinds of derivatized BAs were studied and compared with commercial SPME Arrows. Experimental parameters, e.g., sample volume, derivatization reagent amount, extraction time, and desorption time, which have a dramatic effect on SPME Arrow pretreatment, were optimized. Acidity enhanced MCM-T-H coating showed a much higher affinity to derivatized BAs compared to a commercial SPME Arrow in terms of extraction capacity. In addition, hydrophobicity modification significantly reduced the interference of water molecules on the interaction between MCM-T-H and the derivatized BAs. The MCM-T-H-SPME Arrow showed efficient separation and enrichment capacity for derivatized BAs from complex matrices and therefore, the sample pretreatment time was saved. According to the experimental results, the optimal condition was to add 10 μL derivatization reagent to a 10 mL sample and maintain an agitation speed of 1250 r min−1. The MCM-T-H-SPME showed excellent reproducibility (RSD < 9.8%) and fast adsorption kinetics (30 min) and desorption kinetics (5 min) for derivatized BAs under optimal conditions. In summary, the MCM-T-H-SPME Arrow based method was employed for accurate monitoring of the variations of BAs in pork and fish, and good results were achieved.
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Xu, Ziyan, Chuan Zhou, Haiming Shi, Hong Zhang, Yanlan Bi, and Xuebing Xu. "Processing of Flavor-Enhanced Oils: Optimization and Validation of Multiple Headspace Solid-Phase Microextraction-Arrow to Quantify Pyrazines in the Oils." Life 11, no. 5 (April 26, 2021): 390. http://dx.doi.org/10.3390/life11050390.

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An efficient and effective multiple headspace-solid phase microextraction-arrow-gas chromatography-mass spectrometry (MHS-SPME-arrow-GCMS) analytical protocol is established and used to quantify the flavor compounds in oils. SPME conditions, such as fiber coating, pre-incubation temperature, extraction temperature, and time were studied. The feasibility was compared between SPME-arrow and the traditional fiber by loading different sample amounts. It was found that the SPME-arrow was more suitable for the MHS-SPME. The limit of detection (LODs) and limit of quantitation (LOQs) of pyrazines were in the range of 2–60 ng and 6–180 ng/g oil, respectively. The relative standard deviation (RSD) of both intra- and inter-day were lower than 16%. The mean recoveries for spiked pyrazines in rapeseed oil were in the range of 91.6–109.2%. Furthermore, this newly established method of MHS-SPME-arrow was compared with stable isotopes dilution analysis (SIDA) by using [2H6]-2-methyl-pyrazine. The results are comparable and indicate this method can be used for edible oil flavor analysis.
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Grecco, Caroline Fernandes, Israel Donizeti de Souza, Igor Gustavo Carvalho Oliveira, and Maria Eugênia Costa Queiroz. "In-Tube Solid-Phase Microextraction Directly Coupled to Mass Spectrometric Systems: A Review." Separations 9, no. 12 (November 26, 2022): 394. http://dx.doi.org/10.3390/separations9120394.

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Since it was introduced in 1997, in-tube solid-phase microextraction (in-tube SPME), which uses a capillary column as extraction device, has been continuously developed as online microextraction coupled to LC systems (in-tube SPME-LC). In the last decade, new couplings have been evaluated on the basis of state-of-the-art LC instruments, including direct coupling of in-tube SPME to MS/MS systems, without chromatographic separation, for high-throughput analysis. In-tube SPME coupling to MS/MS has been possible thanks to the selectivity of capillary column coatings and MS/MS systems (SRM mode). Different types of capillary columns (wall-coated open-tubular, porous-layer open-tubular, sorbent-packed, porous monolithic rods, or fiber-packed) with selective stationary phases have been developed to increase the sorption capacity and selectivity of in-tube SPME. This review focuses on the in-tube SPME principle, extraction configurations, current advances in direct coupling to MS/MS systems, experimental parameters, coatings, and applications in different areas (food, biological, clinical, and environmental areas) over the last years.
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Herrington, Jason S., German A. Gómez-Ríos, Colton Myers, Gary Stidsen, and David S. Bell. "Hunting Molecules in Complex Matrices with SPME Arrows: A Review." Separations 7, no. 1 (February 15, 2020): 12. http://dx.doi.org/10.3390/separations7010012.

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Thirty years since the invention and public disclosure of solid phase microextraction (SPME), the technology continues evolving and inspiring several other green extraction technologies amenable for the collection of small molecules present in complex matrices. In this manuscript, we review the fundamental and operational aspects of a novel SPME geometry that can be used to “hunt” target molecules in complex matrices: the SPME Arrow. In addition, a series of applications in environmental, food, cannabis and forensic analysis are succinctly covered. Finally, special emphasis is placed on novel interfaces to analytical instrumentation, as well as recent developments in coating materials for the SPME Arrow.
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Chen, Yujun, Tao Gong, Cilong Yu, Xiang Qian, and Xiaohao Wang. "Microfluidic Flow-through SPME Chip for Online Separation and MS Detection of Multiple Analyses in Complex Matrix." Micromachines 11, no. 2 (January 21, 2020): 120. http://dx.doi.org/10.3390/mi11020120.

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Simplifying tedious sample preparation procedures to improve analysis efficiency is a major challenge in contemporary analytical chemistry. Solid phase microextraction (SPME), a technology developed for rapid sample pretreatment, has flexibility in design, geometry, and calibration strategies, which makes it a useful tool in a variety of fields, especially environmental and life sciences. Therefore, it is important to study the coupling between the microfluidic electrospray ionization (ESI) chip integrated with the solid phase microextraction (SPME) module and the electrospray mass spectrometer (MS). In our previous work, we designed a solid phase microextraction (SPME) module on a microfluidic chip through geometric design. However, automation and calibration methods for the extraction process remain unresolved in the SPME on-chip domain, which will lead to faster and more accurate results. This paper discusses the necessity to design a micromixer structure that can produce different elution conditions on the microfluidic chip. By calculating the channel resistances, the microfluidic chip’s integrated module with the micromixer, SPME, and ESI emitters optimize the geometry structure. We propose the annular channel for SPME to perform the resistances balance of the entire chip. Finally, for SPME on a single chip, this work provides a quantitation calibration method to describe the distribution of the analytes between the sample and the extraction phase before reaching the adsorption equilibrium.
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Górecki, Tadeusz, Anna Boyd-Boland, Zhouyao Zhang, and Janusz Pawliszyn. "1995 McBryde Medal Award Lecture Solid phase microextraction – a unique tool for chemical measurements." Canadian Journal of Chemistry 74, no. 7 (July 1, 1996): 1297–308. http://dx.doi.org/10.1139/v96-145.

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The paper presents recent advances in solid phase microextraction (SPME). The method utilizes a small fused silica fibre coated with a suitable polymeric stationary phase for analyte extraction from various matrices. The fibre is mounted in a syringe-like holder for protection. SPME has been used for the characterization of polymeric coating properties. Infinite-dilution weight-fraction activity coefficients have been determined for five solutes in two different stationary phases. Their values correlate well with the structure of the analytes and the coating. Other SPME uses include simultaneous determination of 60 pesticides in liquid matrices. A comparison between SPME, liquid extraction, and Soxhlet extraction for the analysis of Atrazine, Simazine, and Metolachlor in well water, as well as Metolachlor in soil samples, produced similar results for all three methods. The solvent-free character of SPME enables its use as sample introduction technique for fast GC analysis. Separations of BTEX in less than 9 s, and of volatile compounds described in EPA method 624 in 2.5 min, are described. SPME has also been used for the analysis of tetraethyllead and Pb(II) in water. Before the analysis, lead is derivatized with sodium tetraethylborate, and the tetraethyllead formed is extracted from sample headspace. Sub-ppb detection limits have been achieved with FID. Finally, SPME has been coupled to HPLC with the use of a specially designed interface. The combination has been tested on samples of polyaromatic hydrocarbons and surfactants in water. Very good precision of retention times and peak areas has been achieved. Key words: solid phase microextraction, coating characterization, pesticide analysis, fast GC, lead and organolead compounds, SPME/HPLC.
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Segura-Borrego, M. Pilar, Rocío Ríos-Reina, Cristina Ubeda, Raquel M. Callejón, and M. Lourdes Morales. "Comparison of the Novel Thin Film-Solid Phase Microextraction and Sorptive Extraction Methods for Picual and Hojiblanca Olive Oil Volatile Fraction Analysis in Headspace." Foods 9, no. 6 (June 5, 2020): 748. http://dx.doi.org/10.3390/foods9060748.

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For first time, the new device named thin film solid phase microextraction (TF-SPME) has been used to determine the volatile profile of the Picual and Hojiblanca varieties of extra virgin olive oils. To this end, different traditional sampling methods such as headspace sorptive extraction (HSSE) with polydimethylsiloxane (PDMS) and polyethyleneglycol-modified silicone (EG/Silicone) Twisters® have been compared with the TF-SPME devices coated with different extraction polymeric phases. PARADISe software was used as a non-targeting method to process all data. The best results were obtained by HSSE-PDMS and 2TF-SPME. Moreover, the 2TF-SPME extraction method achieved the most adequate results of linearity for most compounds, according to F-values, while the intermediate precision results were similar for both 2TF-SPME and HSSE-PDMS sampling methods. Different sensitivity was observed between both sampling methods depending on the volatile compound, without being clearly influenced by the polarity of them. Although both sampling methods enabled the main active aroma of olive oil to be determined and for them to be differentiated according to olive variety, the 2TF-SPME method appears to be the most suitable for this goal.
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Agatonovic-Kustrin, Snezana, Vladimir Gegechkori, Tamara Kobakhidze, and David Morton. "Solid-Phase Microextraction Techniques and Application in Food and Horticultural Crops." Molecules 28, no. 19 (September 29, 2023): 6880. http://dx.doi.org/10.3390/molecules28196880.

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Solid-phase microextraction (SPME) is a sample preparation technique which utilizes small amounts of an extraction phase for the extraction of target analytes from investigated sample matrices. Its simplicity of use, relatively short sample processing time, and fiber reusability have made SPME an attractive choice for many analytical applications. SPME has been widely applied to the sampling and analysis of environmental, food, aromatic, metallic, forensic, and pharmaceutical samples. Solid phase microextraction is used in horticultural crops, for example, to determine water and soil contaminants (pesticides, alcohols, phenols, amines, herbicides, etc.). SPME is also used in the food industry to separate biologically active substances in food products for various purposes, for example, disease prevention, determining the smell of food products, and analyzing tastes. SPME has been applied to forensic analysis to determine the alcohol concentration in blood and that of sugar in urine. This method has also been widely used in pharmaceutical analysis. It is a solvent-free sample preparation technique that integrates sampling, isolation, and concentration. This review focuses on recent work on the use of SPME techniques in the analysis of food and horticultural crops.
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Tursumbayeva, Madina, Jacek Koziel, Devin Maurer, Bulat Kenessov, and Somchai Rice. "Development of Time-Weighted Average Sampling of Odorous Volatile Organic Compounds in Air with Solid-Phase Microextraction Fiber Housed inside a GC Glass Liner: Proof of Concept." Molecules 24, no. 3 (January 23, 2019): 406. http://dx.doi.org/10.3390/molecules24030406.

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Finding farm-proven, robust sampling technologies for measurement of odorous volatile organic compounds (VOCs) and evaluating the mitigation of nuisance emissions continues to be a challenge. The objective of this research was to develop a new method for quantification of odorous VOCs in air using time-weighted average (TWA) sampling. The main goal was to transform a fragile lab-based technology (i.e., solid-phase microextraction, SPME) into a rugged sampler that can be deployed for longer periods in remote locations. The developed method addresses the need to improve conventional TWA SPME that suffers from the influence of the metallic SPME needle on the sampling process. We eliminated exposure to metallic parts and replaced them with a glass tube to facilitate diffusion from odorous air onto an exposed SPME fiber. A standard gas chromatography (GC) liner recommended for SPME injections was adopted for this purpose. Acetic acid, a common odorous VOC, was selected as a model compound to prove the concept. GC with mass spectrometry (GC–MS) was used for air analysis. An SPME fiber exposed inside a glass liner followed the Fick’s law of diffusion model. There was a linear relationship between extraction time and mass extracted up to 12 h (R2 > 0.99) and the inverse of retraction depth (1/Z) (R2 > 0.99). The amount of VOC adsorbed via the TWA SPME using a GC glass liner to protect the SPME was reproducible. The limit of detection (LOD, signal-to-noise ratio (S/N) = 3) and limit of quantification (LOQ, S/N = 5) were 10 and 18 µg·m−3 (4.3 and 7.2 ppbV), respectively. There was no apparent difference relative to glass liner conditioning, offering a practical simplification for use in the field. The new method related well to field conditions when comparing it to the conventional method based on sorbent tubes. This research shows that an SPME fiber exposed inside a glass liner can be a promising, practical, simple approach for field applications to quantify odorous VOCs.
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Najwa, Lu'luin, Muhammad Iqbal, and Menik Aryani. "Manajemen Implementasi Sistem Penjaminan Mutu Internal di Perguruan Tinggi." Jurnal Visionary : Penelitian dan Pengembangan dibidang Administrasi Pendidikan 11, no. 1 (April 9, 2023): 72. http://dx.doi.org/10.33394/vis.v11i1.7391.

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Sistem Penjaminan mutu di perguruan tinggi ditujukan untuk meningkatkan mutu pendidikan. Perguruan tinggi secara sistematis perlu melaksanakan proses penjaminan mutu yang mengacu pada Standar Nasional Pendidikan Tinggi (SN-Dikti). Sistem penjaminan mutu terbagi menjadi dua, yaitu Sistem Penjaminan Mutu Internal (SPMI) yang dilakukan pihak internal perguruan tinggi secara otonom, sedangkan Sistem Penjaminan Eksternal (SPME) dilakukan oleh pihak luar untuk menentukan kelayakan perguruan tinggi. Penelitian ini bertujuan mendeskripsikan secara jelas tentang sistem penjaminan mutu internal di tingkat perguruan tinggi. Pendekatan yang digunakan dalam penelitian ini adalah literatur review yang bersumber dari dokumen SPMI perguruan tinggi dan kajian artikel dalam jurnal. Hasil penelitian ini adalah berkaitan dengan kebijakan, model manajemen SPMI, prinsip pelaksanaan SPMI, strategi, pelaksanaan dan struktur SPMI. Dengan jelasnya kebijakan dan alur sistem penjaminan internal diharapkan perguruan tinggi dapat mengimplementasikannya dengan bijak.Kata Kunci: Sistem Penjaminan Mutu Internal, Perguruan Tinggi.
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Chen, Jun, Yan Liu, and Juan Hong Gu. "Optimization of SPME with GCMS Analysis of Volatile Organic Chemical Residues in Textiles." Advanced Materials Research 175-176 (January 2011): 559–64. http://dx.doi.org/10.4028/www.scientific.net/amr.175-176.559.

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A fast testing procedure for the determination of VOCs in textile matrix using solid phase microextraction (SPME) and gas chromatography-mass spectrometry (GC-MS) was introduced. Samples were cut into small pieces and soaked in 5% methanol (v/v) saturated NaCl solution with supersonic pretreatment at 40±1°Cwater-bathing for 15 min and headspace exposure for 10 min at 50°C with stirring rate at 1100rmp. The influence of SPME adsorption time, stir speed, adsorption time and temperature, and gas chromatography (GC) inlet conditions for the SPME were investigated. Then the matrix solutions were extracted by headspace SPME and analysis by GC/MS. Under the optimized conditions, the limits of detection for target compounds were 0.005mg/kg with average recovery between 90.6-108.7%. The results obtained clearly showed the potential of SPME for efficient concentration of the target compounds and also demonstrated the reliability of this extraction technique for the monitoring of textile quality for the eco-marks.
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Ahmad, Sheelan, Daniel Baker, Darragh Murnane, Neil Spooner, and Ute Gerhard. "Solid-phase microextraction for assessment of plasma protein binding, a complement to rapid equilibrium dialysis." Bioanalysis 13, no. 14 (July 2021): 1101–11. http://dx.doi.org/10.4155/bio-2021-0109.

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Aim: Determination of plasma protein binding ( PPB) is considered vital for better understanding of pharmacokinetic and pharmacodynamic activities of drugs due to the role of free concentration in pharmacological response. Methodology & results: Solid-phase microextraction (SPME) was investigated for measurement of PPB from biological matrices and compared with a gold standard approach (rapid equilibrium dialysis [RED]). Discussion & conclusion: SPME-derived values of PPB correlated well with literature values, and those determined by RED. Respectively, average protein binding across three concentrations by RED and SPME was 33.1 and 31.7% for metoprolol, 89.0 and 86.6% for propranolol and 99.2 and 99.0% for diclofenac. This study generates some evidence for SPME as an alternative platform for the determination of PPB.
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Cao, Jianping, Li Zhang, Zhibin Cheng, Siqi Xie, Runze Li, Ying Xu, and Haibao Huang. "Quantitative Analysis of Indoor Gaseous Semi-Volatile Organic Compounds Using Solid-Phase Microextraction: Active Sampling and Calibration." Atmosphere 13, no. 5 (April 26, 2022): 693. http://dx.doi.org/10.3390/atmos13050693.

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Semi-volatile organic compounds (SVOCs) are important pollutants in indoor environments. Quantification of gaseous SVOC concentrations is essential to assess the pollution levels. Solid-phase microextraction (SPME) is considered to be an attractive sampling technique with merits, including simplicity of use, rapid sampling, and solvent free. However, the applications of SPME for sampling gaseous SVOCs are often limited by the fluctuating velocity of indoor air (leading to an unstable sampling rate) and the uncertainties associated with the traditional calibration of SPME. Therefore, we established an SPME-based active sampler to ensure the stable sampling of SVOCs in fluctuating air and developed a two-step calibration method based on the sampling principle of SPME. The presented method and a traditional method (sorbent tubes packed with Tenax TA) were simultaneously used to measure SVOC concentrations in an airstream generated in experiments. Three typical indoor SVOCs, diisobutyl phthalate (DiBP), tris (1-chloro-2-propyl) phosphate (TCPP), and benzyl butyl phthalate (BBzP) were chosen as the analytes. Mean concentrations measured by SPME agreed well with the sorbent tubes (relative deviations < 12%), supporting the feasibility of the presented method. Further studies are expected to facilitate the application of the presented method (especially the problem associated with the sampling-tube loss of low volatile SVOCs).
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Ouyang, Gangfeng, and Janusz Pawliszyn. "SPME in environmental analysis." Analytical and Bioanalytical Chemistry 386, no. 4 (May 4, 2006): 1059–73. http://dx.doi.org/10.1007/s00216-006-0460-z.

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PAWLISZYN, JANUSZ, BARBARA PAWLISZYN, and MICHAEL PAWLISZYN. "Solid Phase Microextraction (SPME)." Chemical Educator 2, no. 4 (October 1997): 1–7. http://dx.doi.org/10.1007/s00897970137a.

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Ajmal, Puthiyaveettilparambu Y., Rahul C. Bhangare, Mahesh Tiwari, and Sanjay K. Sahu. "Analysis of Nitroaromatics: A Comparison Between Gas Chromatography, Liquid Chromatography and their Hyphenation with Solid Phase Micro-Extraction." Current Chromatography 6, no. 1 (September 18, 2019): 42–51. http://dx.doi.org/10.2174/2213240606666190423122358.

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Background: A major class of nitro-explosives being used in military and commercial purposes belongs to organic compounds containing nitro (NO2) groups like nitrobenzene, nitrotoluenes, and nitramines. Apart from being energetic materials, these substances are inherently toxic to human beings. These substances may find their way into different environmental matrices from the site of their military or commercial applications. They are present in nature at ultra-trace levels. Methods: Chromatographic techniques have been widely used for the detection and quantification of nitro-explosives from various environmental matrices. The current study involves a comparison of the performance of liquid and gas chromatography with and without pre-concentration techniques like Solid Phase Micro-extraction (SPME) to detect ultra-trace levels nitrobenzene and nitrotoluenes in water. Results: The addition of SPME to chromatographic techniques significantly improves the quality of the analysis in terms of ease and sensitivity. Both SPME-HPLC and SPME-GC are equally competent techniques for the analysis of nitroaromatic explosives from water. Detection limits were improved by upto 5 orders of magnitude by these methods. Conclusion: The methodology for determining nitroaromatic explosives in water samples has been optimized and validated after trying four different methods and comparing their performance. GC and HPLC techniques used alone cannot be sensitive enough to detect these compounds at ultra-trace levels. Both SPME-HPLC-UV and SPME-GC-FID are equally competent techniques. SPME method has been proved to be an excellent tool with no requirement of any tedious sample preparation and chemical processing of the samples.
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Jõul, Piia, Merike Vaher, and Maria Kuhtinskaja. "Carbon aerogel-based solid-phase microextraction coating for the analysis of organophosphorus pesticides." Analytical Methods 13, no. 1 (2021): 69–76. http://dx.doi.org/10.1039/d0ay02002h.

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Liang, Xu, Jian-Hai Wu, Qi-Yue Zhao, Xiu-Ping Dong, Liang Dong, Lei Qin, Xian-Bing Xu, and Ming Du. "Multiple headspace solid-phase micro-extraction for the total content determination of tetramethylpyrazine in various vinegar samples by GC-FID." Analytical Methods 11, no. 18 (2019): 2443–49. http://dx.doi.org/10.1039/c8ay02816h.

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Zhou, Tao, Bei Yang, Haiying Zhang, Yingjia Yu, Bin Chen, Yile Chen, and Gengli Duan. "Identification of Volatile Compounds in Chrysanthemum morifolium by Microwave Distillation Solid-Phase Microextraction Coupled with GC/MS." Journal of AOAC INTERNATIONAL 92, no. 3 (May 1, 2009): 855–61. http://dx.doi.org/10.1093/jaoac/92.3.855.

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Abstract Microwave distillation with concomitant solid-phase microextraction (MD-SPME) coupled with GC/MS was developed for identifying volatile compounds in the dried flowers of Chrysanthemum morifolium (CM). Different experimental parameters, including SPME fiber coating, microwave power, irradiation time, and water volume were optimized. The best results were obtained using carboxen/polydimethylsiloxane fiber with microwave irradiation at 400 W for 3 min and the addition of 1 mL water into 1.0 g sample. The proposed method allowed the isolation, extraction, and concentration of volatile compounds to be completed in a single step. This MD-SPME-GC/MS method has also been compared to the conventional steam distillation method followed by GC/MS for this identification. Thirty-two volatile compounds were identified using the newly developed MD-SPME-GC/MS process. Relative standard deviation values of &lt;9.8 demonstrate good repeatability. In comparison, 27 compounds were identified by traditional steam distillation-GC/MS. Therefore, the proposed MD-SPME-GC/MS method is simple, rapid, and efficient for identifying volatile compounds in CM.
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Báez, Disnelys, Diego Morales, and Jorge A. Pino. "Volatiles from Michelia champaca Flower: Comparative analysis by Simultaneous Distillation-Extraction and Solid Phase Microextraction." Natural Product Communications 7, no. 5 (May 2012): 1934578X1200700. http://dx.doi.org/10.1177/1934578x1200700529.

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The chemical composition of the volatile compounds isolated by simultaneous distillation-extraction (SDE) and headspace-solid phase microextraction (SPME) from flowers of Michelia champaca growing in Cuba was investigated by GC/FID and GC/MS. Sixty-seven and thirty-four components were identified by SDE and SPME, respectively, with 1,8-cineole (22.8%) as the main constituent in the volatile oil isolated by SDE, and methyl benzoate (30.3%), indole (16.6%) and β-elemene (10.4%) the major components detected by SPME.
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Aggarwal, Prashant, James Baker, Mark T. Boyd, Séamus Coyle, Chris Probert, and Elinor A. Chapman. "Optimisation of Urine Sample Preparation for Headspace-Solid Phase Microextraction Gas Chromatography-Mass Spectrometry: Altering Sample pH, Sulphuric Acid Concentration and Phase Ratio." Metabolites 10, no. 12 (November 25, 2020): 482. http://dx.doi.org/10.3390/metabo10120482.

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Headspace-solid phase microextraction gas chromatography-mass spectrometry (HS-SPME-GC-MS) can be used to measure volatile organic compounds (VOCs) in human urine. However, there is no widely adopted standardised protocol for the preparation of urine samples for analysis resulting in an inability to compare studies reliably between laboratories. This paper investigated the effect of altering urine sample pH, volume, and vial size for optimising detection of VOCs when using HS-SPME-GC-MS. This is the first, direct comparison of H2SO4, HCl, and NaOH as treatment techniques prior to HS-SPME-GC-MS analysis. Altering urine sample pH indicates that H2SO4 is more effective at optimising detection of VOCs than HCl or NaOH. H2SO4 resulted in a significantly larger mean number of VOCs being identified per sample (on average, 33.5 VOCs to 24.3 in HCl or 12.2 in NaOH treated urine) and more unique VOCs, produced a more diverse range of classes of VOCs, and led to less HS-SPME-GC-MS degradation. We propose that adding 0.2 mL of 2.5 M H2SO4 to 1 mL of urine within a 10 mL headspace vial is the optimal sample preparation prior to HS-SPME-GC-MS analysis. We hope the use of our optimised method for urinary HS-SPME-GC-MS analysis will enhance our understanding of human disease and bolster metabolic biomarker identification.
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Yang, Yixin, Peige Qin, Xiaoting Zhang, Jiahua Niu, Shufang Tian, Minghua Lu, Jinhua Zhu, and Zongwei Cai. "Layer-by-layer fabrication of g-C3N4 coating for headspace solid-phase microextraction of food additives followed by gas chromatography-flame ionization detection." Analytical Methods 10, no. 3 (2018): 322–29. http://dx.doi.org/10.1039/c7ay02515g.

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Díaz, A., M. T. Galceran, and F. Ventura. "Determination of estrogenic short ethoxy chain nonylphenols and metabolites in river and treated water by SPE (solid phase extraction) and SPME (solid phase microextraction)." Water Supply 3, no. 1-2 (March 1, 2003): 329–34. http://dx.doi.org/10.2166/ws.2003.0121.

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Two solid-phase microextraction (SPME) procedures have been developed to determine short ethoxy chain nonylphenols and metabolites in water. A direct-SPME method has been used for the determination of short ethoxy chain nonylphenols and their brominated derivatives, whereas the in-sample derivatization headspace-SPME method has proved to be suitable for the simultaneous determination of short ethoxy nonylphenols and their acidic metabolites. Several parameters affecting both SPME procedures, such as extraction mode, fiber selection, extraction time, effect of organic modifiers, derivatization reagents and temperature, were optimized. Both methods were able to determine all these compounds at the sub-mg/L level and the results obtained were compared to a solid phase extraction method (SPE). The procedures developed were applied to raw and treated water from Barcelona (NE Spain).
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45

Patel, Dhananjay I., Tuhin Roychowdhury, Collin Jacobsen, Colton Myers, Jason S. Herrington, and Matthew R. Linford. "Evaluation of New, Sputtered Carbon SPME Fibers with a Multi-Functional Group Test Mixture." Separations 8, no. 12 (November 23, 2021): 228. http://dx.doi.org/10.3390/separations8120228.

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We report the first fabrication of sputtered carbon, solid-phase microextraction (SPME) fibers. These fibers have competitive extraction capabilities compared with the commercial carbon wide range (CWR) SPME fiber. This report also includes a demonstration of a newly developed SPME test mix that includes 15 different compounds with a wide range of functional groups and chemical properties. The fiber fabrication process involves sputtering carbon onto fused silica fibers, and the effects of throw distance on the morphology of the carbon coatings were studied. Four different carbon coating thicknesses were evaluated, with PDMS added as a stationary phase. These fibers were characterized with multiple analytical techniques, including scanning electron microscopy (SEM), X-ray photoelectron spectroscopy (XPS), water contact angle (WCA) goniometry, as well as headspace (HS) and direct immersion (DI)–SPME–GC–MS. The best (11.5 µm) sputtered carbon SPME fibers, with and without PDMS, were evaluated using the new evaluation mix and compared with the commercial CWR fiber and a previously sputtered/developed silicon fiber. The new probe mix helped elucidate differences among the fibers, which would have been missed by current commercial test mixes. The sputtered carbon SPME fibers showed similar functional group selectivity as commercial CWR fibers. However, the sputtered carbon fibers showed higher responses per volume compared with the commercial CWR fiber, indicating the porous morphology of the sputtered carbon has the ability to overcome large phase thickness/volume discrepancies and increase the relative recovery for various compounds.
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46

Hendi, Roghayeh, Marzieh Piriyaei, Marzieh Babashpour Asl, and Mir Mahdi Abolghasemi. "Nanoporous Silica-Polypyrrole/SBA-15 as Fiber Coated in the Solid-Phase Microextraction for Determination of Salvia hydrangea DC. Essential Oil." Pharmaceutical Sciences 24, no. 3 (September 23, 2018): 235–39. http://dx.doi.org/10.15171/ps.2018.34.

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Background: In the current study, simultaneous extraction and concentration of the analytes from the headspace on the solid phase microextraction (SPME) fiber were followed by transferring the essential oil components of Salvia hydrangea DC to the headspace with the help of a heating source. Methods: The essential oil components of the plant were extracted and concentrated in a single step. A one-at-the-time optimization procedure was applied to the microextraction conditions by using the nanocomposite fiber of polypyrrole/SBA-15. Results: The results of the essential oil extraction of Salvia hydrangea clearly demonstrated that polypyrrole/SBA-15 fibers were efficient with SPME technique. The acceptable SPME precision in our study was corroborated by the relative standard deviation (RSD) values of less than 15%. Conclusion: In comparison to the hydro-distillation (HD) method, the SPME technique could equally provide monitoring of almost all the constituents of the studied essential oil in an easier way and shorter time with much lower amounts of the plant sample. The results of the essential oil extraction of Salvia hydrangea clearly demonstrated that polypyrrole/SBA-15 fibers were efficient with SPME technique.
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47

Santos, Nathalia Horrana, Julian Zapata, Juan David Dereix, Jhonathan Escobar, Adrielle Borges de Almeida, Fabiano Guimarães Silva, and Mariana Buranelo Egea. "The Active Aroma of “Cerrado” Cashew and Cagaita Fruits: Comparison between Two Extraction Methods." Applied Sciences 12, no. 7 (March 25, 2022): 3330. http://dx.doi.org/10.3390/app12073330.

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The objective of the present work is to characterize the aroma of “Cerrado” cashew (Anacardium othonianum Rizz.) and cagaita (Eugenia dysenterica) pulps. For this, we used headspace (HS) and two extraction methods (solid-phase extraction, SPE and solid-phase microextraction, SPME), as well as gas chromatography-olfactometry (GC-O) and gas chromatography-mass spectrometry (GC-MS) for identification of aroma compounds. While SPME was more efficient and extracted 17 and 21 compounds for “Cerrado” cashew and cagaita pulps, respectively, the SPE method extracted 13 compounds for both pulps. SPME showed higher modified frequency (MF), that is, compounds perceived with higher intensity and by number of judges during olfactometry. On the other hand, the results obtained in this work showed that the extraction techniques seem complementary, since some compounds were not identified by SPE, but were identified by SPME, and vice versa.
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48

Riboni, Fornari, Bianchi, and Careri. "Recent Advances in In Vivo SPME Sampling." Separations 7, no. 1 (January 15, 2020): 6. http://dx.doi.org/10.3390/separations7010006.

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In vivo solid-phase microextraction (SPME) has been recently proposed for the extraction, clean-up and preconcentration of analytes of biological and clinical concern. Bioanalysis can be performed by sampling exo- or endogenous compounds directly in living organisms with minimum invasiveness. In this context, innovative and miniaturized devices characterized by both commercial and lab-made coatings for in vivo SPME tissue sampling have been proposed, thus assessing the feasibility of this technique for biomarker discovery, metabolomics studies or for evaluating the environmental conditions to which organisms can be exposed. Finally, the possibility of directly interfacing SPME to mass spectrometers represents a valuable tool for the rapid quali- and quantitative analysis of complex matrices. This review article provides a survey of in vivo SPME applications focusing on the extraction of tissues, cells and simple organisms. This survey will attempt to cover the state-of- the-art from 2014 up to 2019.
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49

Kenessov, Bulat, Jacek Koziel, Nassiba Baimatova, Olga Demyanenko, and Miras Derbissalin. "Optimization of Time-Weighted Average Air Sampling by Solid-Phase Microextraction Fibers Using Finite Element Analysis Software." Molecules 23, no. 11 (October 23, 2018): 2736. http://dx.doi.org/10.3390/molecules23112736.

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Determination of time-weighted average (TWA) concentrations of volatile organic compounds (VOCs) in air using solid-phase microextraction (SPME) is advantageous over other sampling techniques, but is often characterized by insufficient accuracies, particularly at longer sampling times. Experimental investigation of this issue and disclosing the origin of the problem is problematic and often not practically feasible due to high uncertainties. This research is aimed at developing the model of the TWA extraction process and optimization of TWA air sampling by SPME using finite element analysis software (COMSOL Multiphysics, Burlington, MA, USA). It was established that sampling by porous SPME coatings with high affinity to analytes is affected by slow diffusion of analytes inside the coating, an increase of their concentrations in the air near the fiber tip due to equilibration, and eventual lower sampling rate. The increase of a fiber retraction depth (Z) resulted in better recoveries. Sampling of studied VOCs using 23 ga Carboxen/polydimethylsiloxane (Car/PDMS) assembly at maximum possible Z (40 mm) was proven to provide more accurate results. Alternative sampling configuration based on 78.5 × 0.75 mm internal diameter SPME liner was proven to provide similar accuracy at improved detection limits. Its modification with the decreased internal diameter from the sampling side should provide even better recoveries. The results obtained can be used to develop a more accurate analytical method for determination of TWA concentrations of VOCs in air using SPME. The developed model can be used to simulate sampling of other environments (process gases, water) by retracted SPME fibers.
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50

Yang, Dong-Sik, Zhentian Lei, Mohamed Bedair, and Lloyd W. Sumner. "An Optimized SPME-GC-MS Method for Volatile Metabolite Profiling of Different Alfalfa (Medicago sativa L.) Tissues." Molecules 26, no. 21 (October 27, 2021): 6473. http://dx.doi.org/10.3390/molecules26216473.

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Solid-phase microextraction (SPME) was coupled to gas chromatography mass spectrometry (GC-MS) and a method optimized to quantitatively and qualitatively measure a large array of volatile metabolites in alfalfa glandular trichomes isolated from stems, trichome-free stems, and leaves as part of a non-targeted metabolomics approach. Major SPME extraction parameters optimized included SPME fiber composition, extraction temperature, and extraction time. The optimized SPME method provided the most chemically diverse coverage of alfalfa volatile and semi-volatile metabolites using a DVB/CAR/PDMS fiber, extraction temperature of 60 °C, and an extraction time of 20 min. Alfalfa SPME-GC-MS profiles were processed using automated peak deconvolution and identification (AMDIS) and quantitative data extraction software (MET-IDEA). A total of 87 trichome, 59 stem, and 99 leaf volatile metabolites were detected after background subtraction which removed contaminants present in ambient air and associated with the fibers and NaOH/EDTA buffer solution containing CaCl2. Thirty-seven volatile metabolites were detected in all samples, while 15 volatile metabolites were uniquely detected only in glandular trichomes, 9 only in stems, and 33 specifically in leaves as tissue specific volatile metabolites. Hierarchical cluster analysis (HCA) and principal component analysis (PCA) of glandular trichomes, stems, and leaves showed that the volatile metabolic profiles obtained from the optimized SPME-GC-MS method clearly differentiated the three tissues (glandular trichomes, stems, and leaves), and the biochemical basis for this differentiation is discussed. Although optimized using plant tissues, the method can be applied to other types of samples including fruits and other foods.
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