Artigos de revistas: "SPE-HPLC-MS"

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Chen, Kun-Ming, Ana Calcagnotto, Junjia Zhu, Yuan-Wan Sun, Karam El-Bayoumy e John P. Richie Jr. "Comparison of an HPLC-MS/MS Method with Multiple Commercial ELISA Kits on the Determination of Levels of 8-oxo-7,8-Dihydro-2'-Deoxyguanosine in Human Urine". Journal of New Developments in Chemistry 2, n.º 2 (16 de dezembro de 2018): 1–13. http://dx.doi.org/10.14302/issn.2377-2549.jndc-18-2430.

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Introduction: Analysis of 8-oxodG is usually conducted by either chromatography-based methods or by immunochemical methods commonly used based upon their low cost and high-throughput. However, concern regarding the accuracy of ELISA methods has complicated their use. We directly compare the levels of urinary 8-oxodG obtained by HPLC-MS/MS with three commercially available ELISA kits in this report. Methods: In the current study, a total of 9 human urine samples were analyzed by LC-MS/MS and three commonly used commercial available ELISA kits. Results: We found that urinary 8-oxodG levels analyzed by HPLC-MS/MS [1.4 ± 0.3 nmol/mmol creatinine) were 7.6- to 23.5-fold lower than those detected by ELISA. Overall, the correlations between ELISA and HPLC-MS/MS were poor but were improved after SPE purification for kits from ENZO (P = 0.2817 without SPE; P = 0.0086 with SPE) and Abcam (P = 0.0596 without SPE; P = 0.0473 with SPE). Discussion and conclusion: While we confirmed that SPE purification can improve the correlation between the selected ELISA kits and HPLC-MS/MS, HPLC-MS/MS is still the method of choice to accurately assess the levels of 8-oxodG in human urine.

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Pang, Guo-Fang, Chun-Lin Fan, Feng Zhang, Yan Li, Qiao-Ying Chang, Yan-Zhong Cao, Yong-Ming Liu et al. "High-Throughput GC/MS and HPLC/MS/MS Techniques for the Multiclass, Multiresidue Determination of 653 Pesticides and Chemical Pollutants in Tea". Journal of AOAC INTERNATIONAL 94, n.º 4 (1 de julho de 2011): 1253–96. http://dx.doi.org/10.1093/jaoac/94.4.1253.

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Abstract An effcient and sensitive method has been established for simultaneous determination of 653 pesticides in teas by GC/MS and HPLC/MS/MS. The method involved extraction with acetonitrile followed by cleanup using Cleanert-TPT SPE and subsequent identifcation and quantitation of 490 pesticides by GC/MS and 448 pesticides by HPLC/MS/MS. The LODs for pesticides determined by GC/MS were between 1.0 and 500 µg/kg, and those determined by HPLC/MS/MS were between 0.03 and 4820 µg/kg. At the low fortifcation levels of 0.01–100 µg/kg, the average recoveries of 94% of the pesticides determined by GC/MS were between 60 and 120%, 77% of which had an RSD below 20%. For 91% of pesticides determined by HPLC/MS/MS, the average recoveries were between 60 and 120%, 76% of which had an RSD below 20%. The paper also reports a novel SPE column, Cleanert TPT, which comprised graphitized carbon black (PestiCarb), polyamine silica, and amide polystyrene for purifying the tea samples. The results indicated good repeatiblity and reproducibility.

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Sturm, Sonja, Christina Högner, Christoph Seger e Hermann Stuppner. "Combining HPLC-DAD-QTOF-MS and HPLC-SPE-NMR to Monitor In Vitro Vitetrifolin D Phase I and II Metabolism". Metabolites 11, n.º 8 (9 de agosto de 2021): 529. http://dx.doi.org/10.3390/metabo11080529.

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By combining HPLC-DAD-QTOF-MS and HPLC-SPE-NMR, the in vitro metabolism of vitetrifolin D, a pharmacologically active key molecule from Vitex agnus-castus in liver cell fractions, was investigated. Twenty-seven phase I and phase II metabolites were tentatively identified from the culture broth by HPLC-DAD-QTOF-MS. The subsequent HPLC-SPE-NMR analysis allowed for the unequivocal structural characterization of nine phase I metabolites. Since the preparative isolation of the metabolites was avoided, the substance input was much lower than in conventional strategies. The study did prove that the use of hyphenated instrumental analysis methodologies allows for the successful performance of in vitro metabolism studies, even if the availability of substances is very limited.

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Miao, Hong-Hao, Yi-Nan Wang, Ru-Song Zhao, Wei-Lin Guo, Xia Wang, Ting-Ting Shen, Chen Wang e Xi-Kui Wang. "Determination of triclocarban in aquatic plants by using SPE combined with HPLC-ESI-MS/MS". Anal. Methods 6, n.º 7 (2014): 2227–32. http://dx.doi.org/10.1039/c3ay42304b.

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A convenient and reliable analytical method was developed for determination of antibacterial triclocarban in aquatic plants based on homogenate extraction, SPE clean-up, and HPLC-ESI-MS/MS determination.

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Lee, Sunmin, Dong-Gu Oh, Digar Singh, Hye Jin Lee, Ga Ryun Kim, Sarah Lee, Jong Seok Lee e Choong Hwan Lee. "Untargeted Metabolomics Toward Systematic Characterization of Antioxidant Compounds in Betulaceae Family Plant Extracts". Metabolites 9, n.º 9 (16 de setembro de 2019): 186. http://dx.doi.org/10.3390/metabo9090186.

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Plant species have traditionally been revered for their unparalleled pharmacognostic applications. We outline a non-iterative multi-parallel metabolomic-cum-bioassay-guided methodology toward the functional characterization of ethanol extracts from the Betulaceae family plants (n = 10). We performed mass spectrometry (MS)-based multivariate analyses and bioassay-guided (ABTS antioxidant activity and cytoprotective effects against H2O2-induced cell damage) analyses of SPE fractions. A clearly distinct metabolomic pattern coupled with significantly higher bioactivities was observed for 40% methanol SPE eluate. Further, the 40% SPE eluate was subjected to preparative high-performance liquid chromatography (prep-HPLC) analysis, yielding 72 sub-fractions (1 min−1), with the highest antioxidant activities observed for the 15 min and 31 min sub-fractions. We simultaneously performed hyphenated-MS-based metabolite characterization of bioactive components for both the 40% methanol SPE fraction and its prep-HPLC sub-fraction (15 min and 31 min). Altogether, 19 candidate metabolites were mainly observed to contribute toward the observed bioactivities. In particular, ethyl gallate was mainly observed to affect the antioxidant activities of SPE and prep-HPLC fractions of Alnus firma extracts. We propose an integrated metabolomic-cum-bioassay-guided approach for the expeditious selection and characterization of discriminant metabolites with desired phenotypes or bioactivities.

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Kovalczuk, T., J. Poustka e J. Hajšlová. "HPLC-MS/MS method for analysis of isoproturon in difficult matrix: poppy seeds". Czech Journal of Food Sciences 26, No. 2 (17 de abril de 2008): 146–52. http://dx.doi.org/10.17221/2469-cjfs.

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While several validated methods have been developed for analysis of phenylurea herbicides in staple food plants, analytical procedures suitable for their quantification in minor crops such as poppy seeds are not available. For the registration of isoproturon use in this crop, the documentation of dynamics of its residues following treatment was requested. To accomplish this task, HPLC-MS/MS method was developed. Extraction of residues was realised by methanol-water mixture, Supelclean LC-18 SPE cartridges were used for purification of crude extracts. For HPLC separation of isoproturon SPE fraction Lichrospher C18 column (25 cm × 4 mm, 5 μm) was employed. For detection and quantification of target analyte, mass spectrometer with ion trap analyser operated in positive atmospheric pressure chemical ionisation (APCI) and MS/MS mode was used. Following performance parameters of method were obtained: detection limit 0.01 mg/kg, recovery 84%, and repeatability 7%.

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Liu, Lei, Yabin Wen, Kangning Liu, Liang Sun, Yaxin Lu e Zheng Yin. "Simultaneous determination of a broad range of cardiovascular drugs in plasma with a simple and efficient extraction/clean up procedure and chromatography-mass spectrometry analysis". RSC Adv. 4, n.º 38 (2014): 19629–39. http://dx.doi.org/10.1039/c4ra01045k.

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A simple, easy to use and efficient method was described for simultaneous determination of ten cardiovascular drugs with a broad range of physicochemical properties in rat plasma via online SPE and HPLC-MS/MS.

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Verma, Kusum S., e Kang Xia. "Analysis of Triclosan and Triclocarban in Soil and Biosolids Using Molecularly Imprinted Solid Phase Extraction Coupled with HPLC-UV". Journal of AOAC INTERNATIONAL 93, n.º 4 (1 de julho de 2010): 1313–21. http://dx.doi.org/10.1093/jaoac/93.4.1313.

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Abstract A molecularly imprinted polymer (MIP) able to selectively bind triclosan (TCS) and triclocarban (TCC), commonly used antibacterial agents in many consumer products, was prepared using noncovalent molecular imprinting methods. The prepared MIP was evaluated as a selective sorbent in SPE for sample cleanup before HPLC-UV analysis of TCS and TCC in soil and biosolid samples. The MIP was also compared with commercially available C18 SPE sorbent. The molecularly imprinted SPE (MISPE) developed in this study was more efficient than C18 SPE for the cleanup of extracts of soil and biosolid samples prior to the analysis of TCC and TCS using HPLC-UV. The LOQ values for both TCC and TCS in the soil samples were determined to be 40 g/kg; in the biosolid samples, the LOQ values were 100 and 300 g/kg for TCC and TCS, respectively. Compared to C18 SPE, using MISPE for sample cleanup may result in a significant reduction of analytical cost, because one MIP can be reused up to 35 times and HPLC-UV instead of HPLC/MS can be used for instrumental analysis following sample cleanup by MISPE.

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Londonio, Agustín, Paul Emir Hasuoka, Pablo Pacheco, Raúl Andrés Gil e Patricia Smichowski. "Online solid phase extraction-HPLC-ICP-MS system for mercury and methylmercury preconcentration using functionalised carbon nanotubes for their determination in dietary supplements". Journal of Analytical Atomic Spectrometry 33, n.º 10 (2018): 1737–44. http://dx.doi.org/10.1039/c8ja00188j.

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Palagama, Dilrukshika S. W., Raymond E. West III e Dragan Isailovic. "Improved solid-phase extraction protocol and sensitive quantification of six microcystins in water using an HPLC-orbitrap mass spectrometry system". Analytical Methods 9, n.º 13 (2017): 2021–30. http://dx.doi.org/10.1039/c6ay03459d.

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Cappiello, Achille, Arnaldo Berloni, Giorgio Famiglini, Filippo Mangani e Pierangela Palma. "Micro-SPE Method for Sample Introduction in Capillary HPLC/MS". Analytical Chemistry 73, n.º 2 (janeiro de 2001): 298–302. http://dx.doi.org/10.1021/ac000859z.

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Wang, Xiaoli, Tao Guo, Yunbo Wei, Guiju Xu, Na Li, Jinhong Feng e Rusong Zhao. "Determination of Quinolone Antibiotic Residues in Human Serum and Urine Using High-Performance Liquid Chromatography/Tandem Mass Spectrometry". Journal of Analytical Toxicology 43, n.º 7 (16 de maio de 2019): 579–86. http://dx.doi.org/10.1093/jat/bkz034.

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Abstract Quinolone antibiotic residues may pose potential threat to human health. A rapid and sensitive method was developed for the determination of quinolone residues in human serum and urine. After solid phase extraction (SPE) process, eight quinolone residues were analyzed by high-performance liquid chromatography/tandem mass spectrometry (HPLC-MS/MS) using ciprofloxacin-d8 as the internal standard. The relative standard deviation of intra-day and inter-day precision for the eight quinolones were less than 7.52% and the accuracies ranged from 95.8% to 103% in human serum, and from 94.1% to 104% in human urine. The extraction recoveries for the eight quinolones varied from 80.2% to 113% in human serum and 83.4% to 117% in human urine. The limit of detection for the eight quinolones was 0.50–1.00 ng/mL. Quinolone antibiotic residues in human serum and urine from 12 volunteers were successfully analyzed with the validated method. The SPE-HPLC-MS/MS method was useful for accurate determination of quinolone antibiotic residues in human body.

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Sun, Feng Cui, Xue Wen Li, Lin Lin Li, Yan Qiang Ding e Hui Zhao. "Simultaneous Determination of Tetracycline, Macrolide and Sulfonamide Antibiotics in Soils Using Accelerated Solvent Extraction Followed by Solid-Phase Extraction and High Performance Liquid Chromatography Tandem Mass Spectrometry". Advanced Materials Research 718-720 (julho de 2013): 1071–76. http://dx.doi.org/10.4028/www.scientific.net/amr.718-720.1071.

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This research developed and optimized the methods for simultaneous determination of tetracycline (TCs), macrolide (MLs) and sulfonamide (SAs) antibiotics in soils using accelerated solvent extraction (ASE)- solid-phase extraction (SPE)-high performance liquid chromatography tandem mass spectrometry (HPLC-MS/MS). Methanol-citric acid (pH=4.7) was used as extraction solvent, diatomite (washed by EDTA) was used as dispersing agent. Firstly, soil was extracted by ASE with the parameter conditions: pressure 1500 psi, temperature 70°C, static 10 min, 1 circle, then pre-concentration by SPE and followed by HPLC-MS/MS analysis. Recovery was 86.3%~97.4% for SAs, 67.3%~87.4% for TCs and 68.4%~78.3% for MLs. RSD < 9 % and r > 0.99. Limits of detection (LOD) was 0.5~0.9 ug/kg for SAs, 0.2~1.1 ug/kg for TCs and 0.2~0.3 ug/kg for MLs. This method determined 9 kinds of antibiotics within 15 min, the determination accuracy can meet the requirements of actual analysis.

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Ju, Jia Qi, Zhong Hang Wu, Zhen Liu Chen, Zhi Jiang He, Long He, Ze Bin Li e Rong Qng Liang. "Coating Quartz Arc Tube with Polycrystalline Alumina for High Intensity Discharge Lamps". Advanced Materials Research 718-720 (julho de 2013): 219–22. http://dx.doi.org/10.4028/www.scientific.net/amr.718-720.219.

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This research developed and optimized the methods for simultaneous determination of tetracycline (TCs), macrolide (MLs) and sulfonamide (SAs) antibiotics in soils using accelerated solvent extraction (ASE)- solid-phase extraction (SPE)-high performance liquid chromatography tandem mass spectrometry (HPLC-MS/MS). Methanol-citric acid (pH=4.7) was used as extraction solvent, diatomite (washed by EDTA) was used as dispersing agent. Firstly, soil was extracted by ASE with the parameter conditions: pressure 1500 psi, temperature 70°C, static 10 min, 1 circle, then pre-concentration by SPE and followed by HPLC-MS/MS analysis. Recovery was 86.3%~97.4% for SAs, 67.3%~87.4% for TCs and 68.4%~78.3% for MLs. RSD < 9 % and r > 0.99. Limits of detection (LOD) was 0.5~0.9 ug/kg for SAs, 0.2~1.1 ug/kg for TCs and 0.2~0.3 ug/kg for MLs. This method determined 9 kinds of antibiotics within 15 min, the determination accuracy can meet the requirements of actual analysis.

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Wang, Lingling, Yuting Nie, Yujiao Wang, Zhenyu Wang e Bo Xiong. "Qualitative and quantitative determinations of pyridalyl and metabolites in excrement of two representative Lepidoptera pests". RSC Advances 5, n.º 125 (2015): 103474–79. http://dx.doi.org/10.1039/c5ra21984a.

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Qualitative and quantitative SPE followed by HPLC-TOF/MS determination of pyridalyl and its potential metabolites in the excrement of Helicoverpa armigera (H. armigera) and Spodoptera exigua (S. exigua) was developed.

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Fracassetti, Daniela, Ileana Vigentini, Alfredo Lo Faro, Patrizia De Nisi, Roberto Foschino, Antonio Tirelli, Marica Orioli e Marcello Iriti. "Assessment of Tryptophan, Tryptophan Ethylester, and Melatonin Derivatives in Red Wine by SPE-HPLC-FL and SPE-HPLC-MS Methods". Foods 8, n.º 3 (14 de março de 2019): 99. http://dx.doi.org/10.3390/foods8030099.

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Melatonin (MEL) is an indoleamine produced mainly by the pineal gland in vertebrates. It plays a significant role in the regulation of circadian rhythms, mitigation of sleeping disorders, and jet lag. This compound is synthetized from tryptophan (TRP) and it has been found in seeds, fruits, and fermented beverages, including wine. Wine is also a source of other tryptophan derivatives, the tryptophan ethylester (TEE) and MEL isomers (MISs), for which the biological properties need to be elucidated. An analytical method for the simultaneous quantification of TRP, TEE, and MEL was developed by a Solid Phase Extraction (SPE) of a preconcentration of wine followed by high performance liquid chromatography (HPLC) analysis either with fluorescence or mass spectrometer detectors. The analytical method showed a relative standard deviation (RSD) lower than 8%, except for TRP (RSD 10.5% in wine). The recovery was higher than 76%. The versatility of SPE preconcentrations allowed for the adequate preconcentration of wine sample as well as detection of low concentrations, an important aspect especially for MEL (detection limit 0.0023 µg/L). The proposed method proved to be suitable for assessing the investigated compounds in some red wine samples, where 74.4–256.2 µg/L and 0.038–0.063 µg/L of TEE and MEL were detected, respectively. Five MISs were also found in wine samples in concentrations up to 1.97 µg/L.

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Nurfadhila, Lina, Marsah Rahmawati, Nur Komala Fitri, Salsabila Granadha Nibullah e Welly Windari. "Analisis senyawa acetaminophen dalam sampel biologis dengan berbagai macam metode". Journal of Pharmaceutical and Sciences 6, n.º 3 (27 de julho de 2023): 1221–37. http://dx.doi.org/10.36490/journal-jps.com.v6i3.197.

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Acetaminophen atau Paracetamol merupakan senyawa yang memiliki efek farmakologi sebagai analgesik dan antipiretik. Tujuan dari review jurnal ini yaitu guna mengetahui serta memahami berbagai macam metode yang bisa digunakan untuk menganalisis sampel biologis pasien ketika mengkonsumsi paracetamol melalui sampel biologisnya. Proses awal untuk melakukan analisis yaitu dengan melakukan preparasi sampel, sampel-sampel dipreparasi dengan berbagai macam metode yang sesuai seperti, metode ekstraksi cair-cair, ekstraksi fase padat (solid phase extraction (SPE) dan metode presipitasi protein, selanjutnya sampel tersebut akan dianalisis menggunakan instrumen yang tepat seperti, GC-MS, LLE, LC-MS, HPLC-MS, ataupun UHPLC-MS. Dari beberapa instrumen yang digunakan metode HPLC-MS merupakan metode yang paling efektif untuk melakukan analisis sampel biologi, karena HPLC-MS dinilai cepat, selektif dan sensitif serta memiliki LLOQ atau nilai batas bawah kuantifikasi yang paling rendah.

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Wang, Yu, Yuzhen Wang e Huilin Liu. "A Novel Fluorescence and SPE Adsorption Nanomaterials of Molecularly Imprinted Polymers Based on Quantum Dot-Grafted Covalent Organic Frameworks for the High Selectivity and Sensitivity Detection of Ferulic Acid". Nanomaterials 9, n.º 2 (23 de fevereiro de 2019): 305. http://dx.doi.org/10.3390/nano9020305.

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A fluorescence and solid phase extraction (SPE) adsorption nanomaterials of molecularly imprinted polymers (MIPs) based on quantum dot-grafted covalent organic frameworks (QD-grafted COFs) was prepared by one-pot surface-imprinting synthesis method. Amino groups of silane reagent were at the surface of QDs to coordinate COFs efficiently by Schiff-base reactions, providing thermal and chemical stability to MIPs. It also reacted with the phenolic hydroxyl groups of ferulic acid (FA) through non-covalent interactions. The nanomaterials were used as fluorescence sensing and SPE adsorption toward determination of ferulic acid. The MIPs based on QD-grafted COFs had good fluorescence response ability, and quenching linearly at concentrations of ferulic acid from 0.03 to 60 mg kg−1, with a detection limit of 5 µg kg−1. At the same time, it exhibited a good SPE adsorption ability, and the FA extraction was from 1.63 to 3.11 mg kg−1 in grain by-products by SPE coupled with high performance liquid chromatography/mass spectrometry (HPLC/MS). The fluorescence and SPE-HPLC/MS were used for the efficient detection of ferulic acid in real samples with recovery values of 88–114% and 90–97%, respectively. Furthermore, the nanomaterials of MIPs based on QD-grafted COFs were used for FA detection with high sensitivity and selectivity, and it also increased the recycling of waste resources.

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Sun, Xiaojie, Yuanhao Yang, Qiangbing Tian, Derong Shang, Jun Xing e Yuxiu Zhai. "Determination of gentamicin C components in fish tissues through SPE-Hypercarb-HPLC-MS/MS". Journal of Chromatography B 1093-1094 (setembro de 2018): 167–73. http://dx.doi.org/10.1016/j.jchromb.2018.07.011.

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Hernández-Fernández, Joaquín, Heidis Cano e Ana Fonseca Reyes. "Valoration of the Synthetic Antioxidant Tris-(Diterbutyl-Phenol)-Phosphite (Irgafos P-168) from Industrial Wastewater and Application in Polypropylene Matrices to Minimize Its Thermal Degradation". Molecules 28, n.º 7 (2 de abril de 2023): 3163. http://dx.doi.org/10.3390/molecules28073163.

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Industrial wastewater from petrochemical processes is an essential source of the synthetic phenolic phosphite antioxidant (Irgafos P-168), which negatively affects the environment. For the determination and analysis of Irgafos P-168, DSC, HPLC-MS, and FTIR methodologies were used. Solid phase extraction (SPE) proved to be the best technique for extracting Irgafos from wastewater. HPLC-MS and SPE determined the repeatability, reproducibility, and linearity of the method and the SPE of the standards and samples. The relative standard deviations, errors, and correlation coefficients for the repeatability and reproducibility of the calibration curves were less than 4.4% and 4.2% and greater than 0.99955, respectively. The analysis of variance (ANOVA), using the Fisher method with confidence in 95% of the data, did not reveal significant differences between the mentioned parameters. The removal of the antioxidant from the wastewater by SPE showed recovery percentages higher than 91.03%, and the chemical characterization of this antioxidant by FTIR spectroscopy, DSC, TGA, and MS showed it to be structurally the same as the Irgafos P-168 molecule. The recovered Irgafos was added to the polypropylene matrix, significantly improving its oxidation times. An OIT analysis, performed using DSC, showed that the recovered Irgafos-blended polypropylene (PP) demonstrated oxidative degradation at 8 min. With the addition of the Irgafos, the oxidation time was 13 min. This increases the polypropylene’s useful life and minimizes the environmental impact of the wastewater.

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Wang, Bo, Jianyu Liu, Xia Zhao, Kaizhou Xie, Zhixiang Diao, Genxi Zhang, Tao Zhang e Guojun Dai. "Determination of Eight Coccidiostats in Eggs by Liquid–Liquid Extraction–Solid-Phase Extraction and Liquid Chromatography–Tandem Mass Spectrometry". Molecules 25, n.º 4 (22 de fevereiro de 2020): 987. http://dx.doi.org/10.3390/molecules25040987.

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A method for the simultaneous determination of robenidine, halofuginone, lasalocid, monensin, nigericin, salinomycin, narasin, and maduramicin residues in eggs by liquid chromatography–tandem mass spectrometry (LC–MS/MS) was developed. The sample preparation method used a combination of liquid–liquid extraction (LLE) and solid-phase extraction (SPE) technology to extract and purify these target compounds from eggs. The target compounds were separated by gradient elution using high-performance liquid chromatography (HPLC) and ultra-performance liquid chromatography (UPLC). Tandem mass spectrometry was used to quantitatively and qualitatively analyze the target compounds via electrospray ionization (ESI+) and multiple reaction monitoring mode. The HPLC–MS/MS and UPLC–MS/MS methods were validated according to the requirements defined by the European Union and the Food and Drug Administration. The limits of detection and limits of quantification of the eight coccidiostats in eggs were 0.23–0.52 µg/kg and 0.82–1.73 µg/kg for HPLC–MS/MS, and 0.16-0.42 µg/kg and 0.81-1.25 µg/kg for UPLC–MS/MS, respectively. The eggs were spiked with four concentrations of the eight coccidiostats, and the HPLC–MS/MS and UPLC–MS/MS average recoveries were all higher than 71.69% and 72.26%, respectively. Compared with the HPLC–MS/MS method, utilizing UPLC–MS/MS had the advantages of low reagent consumption, a short detection time, and high recovery and precision. Finally, the HPLC–MS/MS and UPLC–MS/MS methods were successfully applied to detect eight coccidiostats in 40 eggs.

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Fu, Jiang, Ya-Nan Wang, Shuang-Gang Ma, Li Li, Xiao-Jing Wang, Yong Li, Yun-Bao Liu, Jing Qu e Shi-Shan Yu. "Xanthanoltrimer A–C: three xanthanolide sesquiterpene trimers from the fruits of Xanthium italicum Moretti isolated by HPLC-MS-SPE-NMR". Organic Chemistry Frontiers 8, n.º 6 (2021): 1288–93. http://dx.doi.org/10.1039/d0qo01541e.

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Xanthanoltrimer A–C, first three xanthanolide sesquiterpene trimers from the fruits of Xanthium italicum Moretti, were isolated by HPLC-MS-SPE-NMR. Xanthanoltrimer A–C had an unprecedented 5/7/6/5/7/6/5/7 polycyclic scaffold.

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Sorokin, A. V., e V. V. Ovcharenko. "LC-MS/MS Analysis of Glyphosate, Aminomethylphosphonic acid and Glufosinate in Honey". Asian Journal of Chemistry 34, n.º 8 (2022): 2128–32. http://dx.doi.org/10.14233/ajchem.2022.23801.

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A confirmatory method was developed and validated for determination of glyphosate (Gly), glufosinate (Glu) and aminomethylphosphonic acid (AMPA) in honey using reversed-phase high performance liquid chromatography (RP-HPLC) coupled with tandem mass-spectrometry (MS/MS). The sample preparation approach consists of extraction by acidified solutions followed by SPE on Oasis HLB, derivatization by FMOC-Cl, concentration and another SPE stage on Oasis WCX. The limit of quantification (LOQ) of 0.05 ppm was reached for Gly, AMPA and Glu. All accuracy values ranged from 85% to 110% for all analytes using both primary and secondary quantitative ion transitions (RSD ≤ 10%). Correlation coefficients were higher than 0.99. The method was applied in 2018-19 for monitoring of honey samples, which revealed agricultural territories with intensive use of glyphosate.

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Wu, Jianbing, Linyao Chen, Peipei Mao, Yanbin Lu e Huizhong Wang. "Determination of chloramphenicol in aquatic products by graphene-based SPE coupled with HPLC-MS/MS". Journal of Separation Science 35, n.º 24 (dezembro de 2012): 3586–92. http://dx.doi.org/10.1002/jssc.201200617.

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Tuzimski, Tomasz, Szymon Szubartowski, Renata Gadzała-Kopciuch, Andrzej Miturski, Monika Wójtowicz-Marzec, Wojciech Kwaśniewski e Bogusław Buszewski. "Comparison of DAD and FLD Detection for Identification of Selected Bisphenols in Human Breast Milk Samples and Their Quantitative Analysis by LC-MS/MS". Journal of AOAC INTERNATIONAL 103, n.º 4 (28 de fevereiro de 2020): 1029–42. http://dx.doi.org/10.1093/jaoacint/qsaa027.

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Abstract Background Determination of bisphenols released from packaging material is undoubtedly a difficult and tricky task, requiring the chemical analyst to develop an individual approach to obtain reliable analytical information. Objective QuECHERS (Quick, Easy, Cheap, Effective, Rugged, and Safe)/dispersive solid-phase extraction (d-SPE) technique and high performance liquid chromatography (HPLC) coupled with modern detection techniques such as diode-array detector (DAD), ﬂuorescence detector (FLD) or tandem mass spectrometry (MS/MS) for the determination of bisphenols such as bisphenol A (BPA), bisphenol S (BPS), bisphenol F (BPF), bisphenol B (BPB), 2-[[4-[2-[4-(Oxiran-2-ylmethoxy)phenyl]propan-2yl]phenoxy] methyl]oxirane (BADGE), 3-[4-[2-[4-(Oxiran-2-ylmethoxy)phenyl]propan-2-yl]phenoxy]propane-1,2-diol (BADGE*H2O), 3-[4-[2-[4-(2,3-Dihydroxypropoxy)phenyl]propan-2-yl]phenoxy]propane-1,2-diol (BADGE*2H2O), 1-Chloro-3-[4-[2-[4-(3-chloro-2-hydroxypropoxy)phenyl] propan-2-yl]phenoxy]propan-2-ol (BADGE*2HCl) in human breast milk samples have been performed. Methods For the analysis of total analytes, prior to the extraction with acetonitrile, a deconjugation step was implemented in a tube by adding 1 mL of the enzymatic solution with the β-Glucuronidase to 5 mL of sample. The mix was homogenized and incubated for 17 h at 37°C. Ten milliliters of acetonitrile, and a QuEChERS salt packet with 4 g anhydrous MgSO4 and 1 g NaCl were added. During the d-SPE step the extract was transferred into tube with 30 mg Z-Sep and 50 mg PSA (and also 150 mg MgSO4 for LC-MS/MS analysis). MeOH–water (20:80, v/v) were added to the dry residue and the extract was reconstituted in 150 µL (25-fold analytes pre-concentration is achieved). Next bisphenols were identified by HPLC-DAD-FLD and quantified by LC-MS/MS equipment. Conclusions During the bisphenols HPLC-DAD-FLD analysis, from 6 min a reinforcement of 15 was used, which allowed analytes to be identified at 750 pg/mL. Application of LC-MS/MS allowed quantification of bisphenols in the range from 2.12 to 116.22 ng/mL in a total 27 human breast milk samples. Highlights First QuEChERS/d-SPE coupled with HPLC-DAD-FLD or LC-MS/MS method for the quantification of bisphenols and its analogues in breast milk Faster and cheaper alternative to traditional extraction methods The method was applied for the first biomonitoring of bisphenols and its analogues in breast milk.

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Feng, Yao, Wen-Juan Zhang, Yuan-Wang Liu, Jian-Ming Xue, Shu-Qing Zhang e Zhao-Jun Li. "A Simple, Sensitive, and Reliable Method for the Simultaneous Determination of Multiple Antibiotics in Vegetables through SPE-HPLC-MS/MS". Molecules 23, n.º 8 (6 de agosto de 2018): 1953. http://dx.doi.org/10.3390/molecules23081953.

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Antibiotics, widely used in livestock breeding, enter the environment through animal manure because of incomplete absorption in animals, especially the farmland ecosystem. Therefore, antibiotics may be adsorbed by plants and even become hazardous to human health through the food chain. In this study, a simple, sensitive, and reliable method was developed for the simultaneous determination of eleven antibiotics, including four sulfonamides, two tetracyclines, three fluoroquinolones, tylosin, and chloramphenicol in different vegetable samples using SPE-HPLC-MS/MS. Vegetable samples were extracted by acetonitrile added with hydrochloric acid (125:4, v/v). The extracts were enriched by circumrotating evaporation, and then cleaned through SPE on a hydrophilic-lipophilic balance (HLB) cartridge. All compounds were determined on a C18 reverse phase column through HPLC-MS/MS. The mean recoveries of 11 antibiotics from spiked samples of vegetables ranged from 71.4% to 104.0%. The limits of detection and quantification were 0.06–1.88 μg/kg and 0.20–6.25 μg/kg, respectively. The applicability of this technique demonstrated its good selectivity, high efficiency, and convenience by the analysis of 35 vegetable samples available from a vegetable greenhouse. Antibiotic residues in vegetables have aroused wide concern from the public. Therefore, standards should be established for antibiotic residues in vegetables to ensure food safety and human health.

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Li, Hanle, Jinhai Wu, Jialei Bai, Jianhu Wu e Jin Wu. "Determination of Lincomycin in Milk Using Cu-Based Metal-Organic Framework Adsorbent and Liquid Chromatography-Tandem Mass Spectrometry". Molecules 28, n.º 14 (10 de julho de 2023): 5307. http://dx.doi.org/10.3390/molecules28145307.

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Antibiotic drug residues can adversely affect the human body. Lincomycin is a common veterinary drug that can form residues in foods of animal origin. However, the detection of trace residue levels of lincomycin residues in real samples is challenging. Here, a simple solid phase extraction (SPE) method was developed for the enrichment of lincomycin from cow milk samples before its detection by high-performance liquid chromatography-tandem mass spectrometry (HPLC-MS/MS). The adsorbent used in the SPE was a Cu-based metal-organic framework (Cu-MOF) prepared by the solvothermal synthesis approach. The prepared MOFs were characterized using scanning electron microscopy (SEM), Fourier-transform infrared spectroscopy (FT-IR), X-ray diffractometry (XRD), differential thermogravimetric analysis (TG-DTA), and N2 adsorption-desorption experiments. The adsorption capacity (adsorption equilibrium, extraction time, pH), and elution solvent parameters were investigated. Under the optimized conditions of the HPLC-MS/MS method, lincomycin was detected in the linear range of 10–200 g/L with a detection limit of 0.013 ng/mL. Commercial milk samples were spiked with lincomycin, and a recovery rate between 92.3% and 97.2% was achieved. Therefore, the current method can be successfully applied for the enrichment and determination of lincomycin from milk samples.

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Tuzimski, Tomasz, Tomasz Rejczak, Dominika Pieniążek, Grzegorz Buszewicz e Grzegorz Teresiński. "Comparison of SPE/d-SPE and QuEChERS-Based Extraction Procedures in Terms of Fungicide Residue Analysis in Wine Samples by HPLC–DAD and LC-QqQ-MS". Journal of AOAC INTERNATIONAL 99, n.º 6 (1 de novembro de 2016): 1436–43. http://dx.doi.org/10.5740/jaoacint.16-0277.

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Abstract Two different extraction and clean-up protocols, based on either the SPE/dispersive SPE (d-SPE) or the quick, easy, cheap, effective, rugged, and safe approach, were optimized and compared for determination of six selected fungicides (benalaxyl, metalaxyl, triadimenol, tebuconazole, diniconazole, and epoxiconazole) in wine samples. The pilot study was performed by applying HPLC with diode-array detection, and optimized procedures were easily transferred to the LC triple-quadrupole MS system. Both extraction procedures presented good performance for all the analytes, with recoveries in the range of 70–132% and SDs ≤20%. The d-SPE clean-up step included in both procedures allows obtaining colorless extracts with the majority of coextracted matrix compounds removed. LC with electrospray ionization and tandem MS operating in the multiple reaction monitoring mode provide high sensitivity and selectivity for trace analysis. Both developed procedures were evaluated in terms of commercial wine sample analysis. In three wine samples, metalaxyl and tebuconazole residues were detected at concentrations from 0.14 to 30.7 ng/mL. Both approaches showed satisfactory feasibility for fungicide residue analysis in wine samples.

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Boner, Pamela L., David W. Gottschall e Heasook Kim-Kang. "Determination and Confirmation of Tulathromycin Residues in Bovine Liver and Porcine Kidney via Their Common Hydrolytic Fragment Using High-Performance Liquid Chromatography/Tandem Mass Spectrometry". Journal of AOAC INTERNATIONAL 94, n.º 2 (1 de março de 2011): 436–45. http://dx.doi.org/10.1093/jaoac/94.2.436.

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Abstract An accurate, reliable, and reproducible analytical method using HPLC/MS/MS for the determination of tulathromycin residues in bovine liver and porcine kidney via their common hydrolytic fragment (CP-60,300) was developed and validated. Briefly, the method involved an initial acid treatment of intact tissues, which yielded the common fragment (CP-60,300). A portion of the acid hydrolyzate was purified by SPE using a strong cation exchange cartridge. Evaporation of the purified extract was followed by reconstitution in aqueous buffer and analysis by HPLC/MS/MS under isocratic conditions. The developed method provided acceptable sensitivity for determinative surveillance of tulathromycin in porcine kidney and bovine liver with an LOQ of 7.50 and 2.75 g/g, respectively. The overall recovery and precision (CV) of 45 determinations of each tissue were 97.8 (5.3) for porcine kidney and 96.9 (7.9) for bovine liver. Accuracy, precision, linearity, specificity, and ruggedness were demonstrated. An HPLC/MS/MS method was also developed for use in these tissues as a confirmatory assay following modifications to the MS detection parameters. The confirmatory method demonstrated acceptable sensitivity for confirmatory evaluation of tulathromycin in porcine kidney and bovine liver at tolerances of 15 and 5.5 g/g, respectively.

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Napoletano, Sabino, Camilla Montesano, Dario Compagnone, Roberta Curini, Giuseppe D’ascenzo, Claudia Roccia e Manuel Sergi. "Determination of Illicit Drugs in Urine and Plasma by Micro-SPE Followed by HPLC–MS/MS". Chromatographia 75, n.º 1-2 (21 de outubro de 2011): 55–63. http://dx.doi.org/10.1007/s10337-011-2156-6.

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Tang, Huiru, Chaoni Xiao e Yulan Wang. "Important roles of the hyphenated HPLC-DAD-MS-SPE-NMR technique in metabonomics". Magnetic Resonance in Chemistry 47, S1 (15 de setembro de 2009): S157—S162. http://dx.doi.org/10.1002/mrc.2513.

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Ma, Yuwei, Yuki Hashi, Feng Ji e Jin-Ming Lin. "Determination of phthalates in fruit jellies by dispersive SPE coupled with HPLC-MS". Journal of Separation Science 33, n.º 2 (8 de dezembro de 2009): 251–57. http://dx.doi.org/10.1002/jssc.200900557.

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Cakova, Veronika, Aurélie Urbain, Cyril Antheaume, Nicole Rimlinger, Patrick Wehrung, Frédéric Bonté e Annelise Lobstein. "Identification of Phenanthrene Derivatives inAerides rosea(Orchidaceae) Using the Combined Systems HPLC-ESI-HRMS/MS and HPLC-DAD-MS-SPE-UV-NMR". Phytochemical Analysis 26, n.º 1 (6 de agosto de 2014): 34–39. http://dx.doi.org/10.1002/pca.2533.

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Wang, Yutang, Yuanyuan Liu, Chunxia Xiao, Laping Liu, Miao Hao, Jianguo Wang e Xuebo Liu. "Simultaneous Determination of 15 Phenolic Constituents of Chinese Black Rice Wine by HPLC-MS/MS with SPE". Journal of Food Science 79, n.º 6 (1 de maio de 2014): C1100—C1105. http://dx.doi.org/10.1111/1750-3841.12483.

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Albu, Florin, Iuliana Sora, Florentin Tache, Victor David e Andrei Medvedovici. "On-Line SPE on Restricted Access Adsorbent for HPLC-MS/MS Analysis of Felodipine in Plasma Samples". Analytical Letters 43, n.º 7-8 (4 de maio de 2010): 1330–43. http://dx.doi.org/10.1080/00032710903518740.

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Sergi, Manuel, Natalia Battista, Camilla Montesano, Roberta Curini, Mauro Maccarrone e Dario Compagnone. "Determination of the two major endocannabinoids in human plasma by μ-SPE followed by HPLC-MS/MS". Analytical and Bioanalytical Chemistry 405, n.º 2-3 (31 de julho de 2012): 785–93. http://dx.doi.org/10.1007/s00216-012-6273-3.

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Krynitsky, Alexander J., Steven J. Stout, Huns Nejad e Thomas C. Cavalier. "Multiresidue Determination and Confirmation of Imidazolinone Herbicides in Soil by High-Performance Liquid Chromatography/Electrospray Ionization Mass Spectrometry". Journal of AOAC INTERNATIONAL 82, n.º 4 (1 de julho de 1999): 956–62. http://dx.doi.org/10.1093/jaoac/82.4.956.

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Abstract A new multiresidue method was developed to determine 6 imidazolinone herbicides in 5 different soil types, using high-performance liquid chromatography/electrospray ionization mass spectrometry (HPLC/ESMS). Good recoveries and sensitivity were obtained for the compounds investigated at the 2.0 ppb limit of quantitation. A 50 g portion of soil was extracted with 0.5N NaOH. A portion of the extract was acidified to precipitate humic acids, and the supernatant was loaded onto a preconditioned tC-18 solid-phase extraction (SPE) cartridge and eluted with ethyl acetate. Further cleanup was achieved by using a tandem strong-anion-ex- change SPE/strong-cation-exchange (SCX) SPE. Analytes were eluted from the SCX SPE with saturated KCI in methanol. After cleanup, the sample was desalted with an RP-102 SPE cartridge. Quantitation was achieved by monitoring the [M + H]+ ions for each compound, with a time-scheduled selective-ion-monitoring program (positive mode). The extraction and cleanup procedure produced a purified extract for MS confirmation using 3 ions with “in-source” collision-induced dissociation.

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Chang, C. C., e S. S. Lee. "Rapid identification of flavonoid glycosides in Pasania kawakamii and Cyclobalanopsis morii via HPLC/MS and HPLC-SPE-NMRa". Chemistry of Natural Compounds 48, n.º 4 (setembro de 2012): 689–92. http://dx.doi.org/10.1007/s10600-012-0352-8.

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Wróblewski, Karol, Anna Petruczynik, Tomasz Tuzimski, Dominika Przygodzka, Grzegorz Buszewicz, Patrycjusz Kołodziejczyk e Piotr Tutka. "Comparison of Various Chromatographic Systems for Analysis of Cytisine in Human Serum, Saliva and Pharmaceutical Formulation by HPLC with Diode Array, Fluorescence or Mass Spectrometry Detection". Molecules 24, n.º 14 (16 de julho de 2019): 2580. http://dx.doi.org/10.3390/molecules24142580.

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Background: Identification and quantitative determination of cytisine, especially in biological samples and pharmaceutical formulations, is still a difficult analytical task. Cytisine is an alkaloid with a small and very polar molecule. For this reason, it is very weakly retained on reversed phase (RP) stationary phases, such as commonly used alkyl-bonded phases. The very weak retention of cytisine causes it to be eluted together with the components of biological matrices. Objective: Comparison and evaluation of various chromatographic systems for analysis of cytisine in different matrices—serum, saliva and pharmaceutical formulation—by high performance liquid chromatography (HPLC) with diode array (DAD), fluorescence (FLD) and mass spectrometry (MS) detection. Methods: The analyses were performed using HPLC in reversed phase (RP), hydrophilic interaction liquid chromatography (HILIC) and ion exchange chromatography (IEC) modes. Different sample pre-treatment methods were tested: Protein precipitation (with acetone, methanol (MeOH) or acetonitrile (ACN), and solid phase extraction (SPE) using cartridges with octadecyl (C18), hydrophilic-lipophilic balanced copolymer (HLB) or strong cation exchange sorbents (Strata X-C). Conclusion: Significant differences were observed in retention parameters with a change of the used chromatographic system. The various properties of stationary phases resulted in differences in analyte retention, peaks’ shape and systems’ efficiency. The weakest retention was observed using RP systems; however, the use of the Polar RP phase can be an alternative for application in green chromatography. In the strongest retention was observed using a strong cation exchange (SCX) phase. The most optimal systems were chosen for the analysis of cytisine in the pharmaceutical preparation, serum and saliva after sample pre-treatment with the new SPE procedure. Due to the sensitivity, the use of HPLC-DAD or HPLC-FLD is the most optimal for drug analysis in pharmaceutical preparations, whereas HPLC-MS is suitable for analysis of cytisine in biological samples.

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Kizaibek, Murat, Ruxandra Popescu, Sonja Prinz, Halmurat Upur, Judith Singhuber, Martin Zehl e Brigitte Kopp. "Towards Modernization of the Formulation of the Traditional Uighur Medicine Herbal PreparationAbnormal Savda Munziq". Evidence-Based Complementary and Alternative Medicine 2012 (2012): 1–10. http://dx.doi.org/10.1155/2012/863101.

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Abnormal Savda Munziq(ASMq) is a herbal preparation used in Traditional Uighur Medicine for the treatment and prevention of diabetes, cardiovascular diseases, chronic asthma and cancer. The recommended dose of this decoction for cancer patients is 500 mL administered orally three times a day. Our approach aimed at reducing the high amount of fluid intake required by fractionation of ASMq guided by the antiproliferative activity on HL-60 cells. The fractionation of ASMq resulted in the preparation of an active extract, Extr-4. Using solid phase extraction, Extr-4 was further fractionated into five fractions (SPE-0, SPE-20, SPE-40, SPE-60 and SPE-80), with SPE-40 showing the strongest antiproliferative activity. Caffeic acid, rutin, isoquercitrin, isorhamnetin 3-O-rutinoside, apigenin 7-O-glucoside, rosmarinic acid, luteolin and formononetin were identified in Extr-4 and fractions thereof by means of TLC, HPLC-DAD and LC-MS. SPE-40 contained the main compounds responsible for the antiproliferative activity on HL-60 cells. Thus, a phenolic fraction with high antiproliferative activity on HL-60 cells was obtained from ASMq through the bioassay-guided fractionation process. This could provide a better pharmaceutical formulation that minimizes the administration inconveniencies of a high volume (1.5 L per day) of ASMq decoction for cancer patients.

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Chen, Lan, Zhaoyuan He, Peiyang Zhang, Yawen Guo, Yang Lu, Yayun Tang, Jinyuan Chen e Kaizhou Xie. "Simultaneous Determination of Levamisole, Mebendazole, and the Two Metabolite Residues of Mebendazole in Poultry Eggs by High-Performance Liquid Chromatography–Tandem Mass Spectrometry". Separations 9, n.º 4 (24 de março de 2022): 83. http://dx.doi.org/10.3390/separations9040083.

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The quantitative determination of levamisole (LMS), mebendazole (MBZ), and the two metabolites of MBZ, 5-hydroxymebendazole (HMBZ) and 2-amino-5-benzoylbenzimidazole (AMBZ), in poultry eggs (hen, duck, and goose) was achieved with high-performance liquid chromatography–tandem triple quadrupole mass spectrometry (HPLC–MS/MS). Samples were pretreated by liquid–liquid extraction and solid-phase extraction (LLE–SPE) to extract the target compounds, and an Oasis MCX SPE column was used for purification. Determination was performed on an Xbridge C18 column with 0.1% formic acid aqueous solution and acetonitrile as mobile phases. LMS, MBZ, HMBZ, and AMBZ were detected in a triple-quadrupole mass spectrometer with ESI in positive mode and quantified with an external standard. In blank eggs, the target analyte concentrations were within the limits of quantification (LOQs)—25 μg/kg (LMS) and 150 μg/kg (MBZ, HMBZ, and AMBZ)—and the matrix-matched calibration curves had good linearity (R2 ≥ 0.9990). In the same concentration range, the average recoveries of the target analytes were 85.98–97.38% (n = 6); the relative standard deviation (RSD), intraday RSD, and interday RSD ranged from 2.06 to 4.22%, 1.40 to 5.85%, and 2.34 to 6.32%, respectively. The limits of detection (LODs) ranged from 0.03 to 0.33 µg/kg, and the LOQs ranged from 0.08 to 1.00 µg/kg. Experimental verification showed that the HPLC–MS/MS method exhibited high specificity and sensitivity for quantitative analyses of egg samples. This study provides a rapid, efficient, and sensitive method for the simultaneous detection of LMS, MBZ, HMBZ, and AMBZ residues in foods of animal origin.

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Liu, Fei, Ya-Nan Wang, Yong Li, Shuang-Gang Ma, Jing Qu, Yun-Bao Liu, Chang-Shan Niu et al. "Triterpenoids from the twigs and leaves of Rhododendron latoucheae by HPLC‒MS‒SPE‒NMR". Tetrahedron 75, n.º 2 (janeiro de 2019): 296–307. http://dx.doi.org/10.1016/j.tet.2018.11.059.

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Ohoro, Adeniji, Okoh e Okoh. "Distribution and Chemical Analysis of Pharmaceuticals and Personal Care Products (PPCPs) in the Environmental Systems: A Review". International Journal of Environmental Research and Public Health 16, n.º 17 (21 de agosto de 2019): 3026. http://dx.doi.org/10.3390/ijerph16173026.

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PPCPs are found almost everywhere in the environment especially at an alarming rate and at very low concentration in the aquatic systems. Many methods—including pressurized hot water extraction (PHWE), pressurized liquid extraction (PLE), ultrasound-assisted extraction (UAE), and micro-assisted extraction (MAE)—have been employed for their extraction from both surface waters and biota. Solid-phase extraction (SPE) proved to be the best extraction method for these polar, non-volatile, and thermally unstable compounds in water. However, ultrasonic extraction works better for their isolation from sediment because it is cheap and consumes less solvent, even though SPE is preferred as a clean-up method for sediment samples. PPCPs are in groups of—acidic (e.g., diclofenac, ibuprofen, naproxen), neutral (e.g., caffeine, carbamazepine, fluoxetine), and basic pharmaceuticals, as well as antibiotics and estrogens amongst others. PPCPs which are present in trace levels (ng/L) are more often determined by liquid chromatography-mass spectrometry (LC-MS), gas chromatography-mass spectrometry (GC-MS), and high-performance liquid chromatography-ultraviolent (HPLC-UV). Of these, LC-MS and LC-MS-MS are mostly employed for the analysis of this class of compounds, though not without a draw-back of matrix effect. GC-MS and GC-MS-MS are considered as alternative cost-effective methods that can also give better results after derivatization.

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Navarrete, Alicia, M. Paz Martínez-Alcázar, Ignacio Durán, Emiliano Calvo, Belén Valenzuela, Coral Barbas e Antonia García. "Simultaneous online SPE–HPLC–MS/MS analysis of docetaxel, temsirolimus and sirolimus in whole blood and human plasma". Journal of Chromatography B 921-922 (março de 2013): 35–42. http://dx.doi.org/10.1016/j.jchromb.2013.01.017.

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Nebot, Carolina, Patricia Regal, Jose Manuel Miranda, Cristina Fente e Alberto Cepeda. "Rapid method for quantification of nine sulfonamides in bovine milk using HPLC/MS/MS and without using SPE". Food Chemistry 141, n.º 3 (dezembro de 2013): 2294–99. http://dx.doi.org/10.1016/j.foodchem.2013.04.099.

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Gao, Hui, Minli Yang, Minglin Wang, Yansheng Zhao, Ya Cao e Xiaogang Chu. "Determination of 30 Synthetic Food Additives in Soft Drinks by HPLC/Electrospray Ionization-Tandem Mass Spectrometry". Journal of AOAC INTERNATIONAL 96, n.º 1 (1 de janeiro de 2013): 110–15. http://dx.doi.org/10.5740/jaoacint.12-046.

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Abstract A method combining SPE with HPLC/electrospray ionization-MS/MS was developed for simultaneous determination of 30 synthetic food additives, including synthetic colorants, preservatives, and sweeteners in soft drinks. All targets were efficiently separated using the optimized chromatographic and MS conditions and parameters in a single run within 18 min. The LOD of the analytes ranged from 0.01 to 20 μg/kg, and the method was validated with recoveries in the 80.8 to 106.4% range. This multisynthetic additive method was found to be accurate and reliable and will be useful to ensure the safety of food products, such as the labeling and proper use of synthetic food additives in soft drinks.

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Muldianah, Diah, Sulastri Sulastri, Adelia Fatharani, Diany A. Nurdimayanthi, Dinda S. Rahmawati e Hana Fadhilah. "Metode Analisis Paracetamol (Acetaminophen) dalam Darah, Plasma, Dan Serum Manusia". COMSERVA Indonesian Jurnal of Community Services and Development 2, n.º 1 (25 de maio de 2022): 1–12. http://dx.doi.org/10.59141/comserva.v2i1.202.

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Paracetamol (Acetaminophen) is one of the drugs most often prescribed to patients, ranging from children to the elderly, as a pain reliever by inhibiting prostaglandin synthesis in the central nervous system. Paracetamol has a broad therapeutic index with an adult dose of 500-1000 mg each time, with an interval of 4-6 hours. The review article aims to compare the analysis and sample preparation methods used to detect paracetamol in human blood, plasma, and serum. In compiling this article, the search method for research journals via the internet was used with Google. The results obtained showed that the detection of paracetamol in blood and serum was analyzed using the Gas Chromatography-Mass Spectrometry (GC-MS) with SPE (Solid Phase Extraction) sample preparation method while in plasma it was analyzed using several methods, namely Liquid Chromatography-Mass Spectrometry (LC-MS), High-Performance Liquid Chromatography-Mass Spectrometry (HPLC-MS), and Ultra-High-Performance Liquid Chromatography-Mass Spectrometry (UHPLC-MS) with protein precipitation and liquid-liquid extraction sample preparation methods. Among the four methods, the HPLC-MS method is considered fast, selective, and sensitive to analyzing paracetamol

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Rivaro, Paola, Davide Vivado, Carmela Ianni, Annalisa Salis, Alice Parodi e Enrico Millo. "A New Approach to Characterize Siderophore-Type Ligands in Seawater by Solid Phase Synthesis and SPE-HPLC-ESI-MS/MS Analysis". Journal of Marine Science and Engineering 12, n.º 1 (6 de janeiro de 2024): 110. http://dx.doi.org/10.3390/jmse12010110.

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Siderophores are organic ligands involved in dissolved iron (dFe) speciation in the oceans. Their study is crucial for a better understanding of the biogeochemical cycle of Fe in the marine environment, particularly in certain areas, such as the Southern Ocean, where Fe deficiency limits marine productivity. In this study, an analytical method is proposed for the extraction and pre-concentration of siderophores from seawater samples by solid phase extraction (SPE) and subsequent analysis by high-performance liquid chromatography—electrospray ionization—mass spectrometry (HPLC-ESI-MS/MS). Two siderophores were used as standards: Ferrioxamine E, a commercially available hydroxamate siderophore, and a staphyloferrin A-like compound with two citric acid units, synthesized in our laboratories by solid-phase peptide synthesis. A central composite design, considering different pH (2, 3.5, and 5) and sample loading volume (50, 125 and 200 mL) as variables, was used to optimize the extraction yield with SPE C18 cartridges. Tests were conducted on samples of artificial seawater spiked with siderophore standards. Ferrioxamine E showed high extraction yields in all tests carried out. On the contrary, the extraction of staphyloferrin A-like compound was significantly affected by both pH and loading volume.

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Ulusoy, Halil İbrahim, Seren Kilit, Ümmügülsüm Polat, Esra Durgun, Aslıhan Gürbüzer, Elif Tümay Özer e Bilgen Osman. "Sensitive Analysis of Epilepsy Drug, Phenobarbital, Based on Column Type Solid Phase Extraction and HPLC-DAD System". Cumhuriyet Science Journal 45, n.º 4 (30 de dezembro de 2024): 763–68. https://doi.org/10.17776/csj.1572205.

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An analytical approach has been developed for the sensitive determination of Phenobarbital, which is used as an antiepileptic drug molecule. The analysis of this active molecule, which has a very limited study even for its direct determination in the literature review, is mostly done with highly complex device systems such as LC-MS. In analysis with conventional HPLC systems, the limit of detection cannot be in most cases lower than 1 µg mL-1 With this study, a separation and preconcentration method based on solid phase extraction (SPE) was developed for trace phenobarbital molecules, so that even very low concentrations could be monitored. In the proposed method, the target molecules were enriched with column type SPE method, and then their analysis were carried out by with the HPLC-DAD system. As an SPE sorbent, a polymeric material, poly(ethylene glycol dimethacrylate-N-methacryloyl-L-tryptophan methyl ester) [poly(EGDMA-MATrp)], was used in extraction experiments. Experimental variables such as pH of medium, type and amount of desorption solvent, electrolyte effect have been studied and optimized step by step. The linear working range under the optimized conditions were determined in the range of 10.00-400.00 ng mL-1 with the limit of detection as 3.57 ng mL-1. Quantitative results were obtained in recovery experiments with the help of model solutions including phenobarbital molecule

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Rudakov, Yaroslav O., Vladimir F. Selemenev, Ludmila V. Rudakova e Oleg B. Rudakov. "Chromatographic approaches to food quality control by chemical compo-sition". Сорбционные и хроматографические процессы 24, n.º 2 (28 de maio de 2024): 197–208. http://dx.doi.org/10.17308/sorpchrom.2024.24/12125.

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The article provides an overview of chromatographic methods, which, when used comprehensively, ensure food quality control and safety. It considers gas chromatography methods that allow analysing volatile components in products using a flame ionization detector, an electron capture detector, and mass-selective detectors (GC-FID, GC-ECD, GC-MS, and GC-MS/MS). The article provides a list of analytes that can be detected by high performance liquid chromatography in combination with refractometric, spectrometric, and mass selective detectors (HPLC-RMD, HPLC-UV, HPLC-SPD, HPLC-MS, and HPLC-MS/MS). The study showed how ion chromatography and capillary electrophoresis with electrochemical detectors (IC-ECD, CE-ECD) can be used to detect ionogenic compounds. It highlighted the importance of thin layer chromatography (TLC) in combination with optical digital colour recording devices in the qualitative and quantitative analysis of contaminants in food products. Since it has been established that micro- and nanoplastics have a negative impact on human health, it is very important to detect these particles in food products. This task can be solved by using gel permeation chromatography (GPC) and hydrodynamic chromatography (HDC), as well as the method of field-flaw fractionation (FFF). It was shown that the GC-MS method is now becoming a priority instrumental method used in accredited analytical laboratories to identify impurities of contaminants in agricultural products. The pyrolytic GC-MS method is promising in this regard. The pyrolytic cell does not require the transfer of a solid sample into a solution for its analysis. The paper considers extraction and sorption methods for the preparation of samples for chromatographic analysis. A variety of liquid-liquid extraction (LLE) and solid-phase extraction (SPE.) methods are most commonly used. Recently, the QuEChERS method has been developed and widely implemented. The overview is primarily based on the papers dedicated to chromatography and related separation methods published by researchers belonging to Voronezh scientific schools.

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