Articoli di riviste: "SPE-HPLC-MS/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. 2 (16 dicembre 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. 4 (1 luglio 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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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. 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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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 aprile 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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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. 8 (9 agosto 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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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. 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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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 (settembre 2018): 167–73. http://dx.doi.org/10.1016/j.jchromb.2018.07.011.

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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. 4 (22 febbraio 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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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. 3 (27 luglio 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, 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. 7 (16 maggio 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 (luglio 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 (luglio 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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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. 2 (gennaio 2001): 298–302. http://dx.doi.org/10.1021/ac000859z.

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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. 24 (dicembre 2012): 3586–92. http://dx.doi.org/10.1002/jssc.201200617.

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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. 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. 13 (2017): 2021–30. http://dx.doi.org/10.1039/c6ay03459d.

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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. 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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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. 9 (16 settembre 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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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. 1-2 (21 ottobre 2011): 55–63. http://dx.doi.org/10.1007/s10337-011-2156-6.

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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. 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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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. 4 (28 febbraio 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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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. 2 (1 marzo 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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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. 8 (6 agosto 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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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. 7 (2 aprile 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, 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. 6 (1 maggio 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. 7-8 (4 maggio 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. 2-3 (31 luglio 2012): 785–93. http://dx.doi.org/10.1007/s00216-012-6273-3.

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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. 6 (2021): 1288–93. http://dx.doi.org/10.1039/d0qo01541e.

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Abstract (sommario):

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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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. 14 (10 luglio 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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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. 2 (23 febbraio 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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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. 3 (14 marzo 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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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. 1 (6 agosto 2014): 34–39. http://dx.doi.org/10.1002/pca.2533.

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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. 4 (1 luglio 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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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. 17 (21 agosto 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 (marzo 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. 3 (dicembre 2013): 2294–99. http://dx.doi.org/10.1016/j.foodchem.2013.04.099.

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37

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. 6 (1 novembre 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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Liu, Shaoying, Jicai Fan, Xihui Huang, Quan Jin e Guonian Zhu. "Determination of Sterigmatocystin in Infant Cereals from Hangzhou, China". Journal of AOAC INTERNATIONAL 99, n. 5 (1 settembre 2016): 1273–78. http://dx.doi.org/10.5740/jaoacint.16-0098.

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Abstract A simple method was developed for the determination of sterigmatocystin in infant cereals. The method consists of a quick, easy, cheap, effective, rugged, and safe (QuEChERS) extraction approach and cleanup with an SPE HLB cartridge. After purification for separation and quantification of sterigmatocystin, HPLC with UV detection and diode-array detection (DAD) was used at sterigmatocystin levels >10 μg/kg, whereas ultra-performance LC with electrospray ionization (ESI) and tandem MS (MS/MS) was used at levels <10 μg/kg. The compound was determined by UV-DAD at 325 nm and by ESI-MS/MS in the positive ionization mode. Good r2 values (≥0.99) were found with both UV-DAD and ESI-MS/MS, and satisfactory recoveries (84.8–96.2%) of sterigmatocystin in infant cereals were demonstrated, with RSD values ≤11.43%. The developed analytical method was used for the determination of sterigmatocystin in infant cereals from Hangzhou, China.

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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. 1 (25 maggio 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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40

Hong, Bing, Shen Yu, Min Zhou, Juan Li, Jing Ding e Yong Niu. "Development of a pH-paralleling approach of quantifying six-category pharmaceuticals in surface water using SPE-HPLC-MS/MS". Watershed Ecology and the Environment 3 (2021): 1–16. http://dx.doi.org/10.1016/j.wsee.2021.01.001.

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41

Nehring, Alexandra, Daniel Bury, Hans-Willi Kling, Tobias Weiss, Thomas Brüning e Holger M. Koch. "Determination of human urinary metabolites of the plasticizer di(2-ethylhexyl) adipate (DEHA) by online-SPE-HPLC-MS/MS". Journal of Chromatography B 1124 (agosto 2019): 239–46. http://dx.doi.org/10.1016/j.jchromb.2019.06.019.

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42

Stepan, Herwig, Jutta Pani, Stefan Pummer, Maria-Theres Weber, Ludwig Hofbauer, Georg Pour, Bernhard Mayer-Helm e Madeleine Werneth. "Sensitive Determination of Ethyl Carbamate in Smokeless Tobacco Products and Cigarette Smoke Using SPE and HPLC–APCI–MS/MS". Chromatographia 78, n. 9-10 (25 febbraio 2015): 675–81. http://dx.doi.org/10.1007/s10337-015-2871-5.

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43

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 settembre 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. 2 (8 dicembre 2009): 251–57. http://dx.doi.org/10.1002/jssc.200900557.

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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. 1 (1 gennaio 2013): 110–15. http://dx.doi.org/10.5740/jaoacint.12-046.

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Abstract (sommario):

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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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. 1 (6 gennaio 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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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. 2 (28 maggio 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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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. 4 (24 marzo 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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Cheng, Yan, Hui Ming Chen, Wei Chen, Yuan Cui, Xiao Juan Li, Dong Dong Chen, Shu Juan Li, Wen Lian Yu e Xin Zhou. "Determination of Perfluorooctane Sulfonates (PFOS) in Four Chemical Materials by HPLC/MS/MS". Advanced Materials Research 554-556 (luglio 2012): 1872–79. http://dx.doi.org/10.4028/www.scientific.net/amr.554-556.1872.

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Abstract (sommario):

A rapid method based on high performance liquid chromatography-tandem mass spectrometry (HPLC/MS/MS) with accelerated solvent extraction (ASE) or solid phase extraction (SPE) was developed for quantitative determination of perfluorooctane sulfonate (PFOS) in the coatings of nonstick pot, food packaging materials, waterborne coatings containing fluoride and fire-fighting foams. The linear calibration curve was obtained in the range of 0.002 - 0.1 μg/mL with a linear correlation coefficient (R2) of 0.998 or 0.999. The recovery for PFOS was in the range of 93.4 - 103% with relative standard deviation of 0.48 - 3.59%. The detection limit for PFOS was 0.4 μg/m2 with a signal-to-noise ratio of 10 for the coatings of nonstick pot and the food packaging materials, and 0.0002% for waterborne coatings containing fluoride and fire-fighting foams, both of which meet the restriction requirement for PFOS content in these chemical materials and consumer products in the EU directives.

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Gorassini, Andrea, Giancarlo Verardo, Scharina-Carol Fregolent e Renzo Bortolomeazzi. "Rapid determination of cholesterol oxidation products in milk powder based products by reversed phase SPE and HPLC-APCI-MS/MS". Food Chemistry 230 (settembre 2017): 604–10. http://dx.doi.org/10.1016/j.foodchem.2017.03.080.

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