Toxicologie Analytique et Clinique
·
2025
·
IF 1.7
Jiajun Sun,Xiaolong Zhang,Mengchao Wang,Xiaoyu Zhou,Yuxuan Chen,Jinlei liu,Yinyin Dai,Kundi Zhao,Yaqin Sun,Jie Gu,Huimin Zhang,Shengnan Zhang,Amin Wurita,Koutaro Hasegawa
Purpose Fluoxetine is a clinically used antidepressant, due to its slimming effect, unscrupulous elements will add it to slimming products. The aim of this study was to establish an optimized derivatization method for fluoxetine and norfluoxetine to be analized by a gas chromatography-tandem mass spectrometry (GC-MS/MS) and apply it to real case. Methods Hair samples were washed and cut into approximately 2 mm, and 50 mg was added to the internal standard and hydrolyzed with 1% sodium hydroxide solution. Add 3 mL ethyl acetate, vortex and centrifuge; urine samples were taken as 1 mL and then added to the internal standard and 3 mL ethyl acetate, then submitted to vortex and centrifugation. The supernatant was evaporated to dryness under a nitrogen gas stream and then derivatized by adding 25 μL ethyl acetate and 25 μL HFBA at 70 °C for 45 minutes and later analyzed by GC-MS/MS. The derivatisation procedure for the remaining derivatisation reagents TFAA, FPPA, MSTFA and 99% BSTFA + 1% TMCS was the same as above. Result Fluoxetine and norfluoxetine were analyzed by GC-MS/MS and the validation data were satisfactory. The derivatization reagent HFBA was the most effective for the modification of fluoxetine and norfluoxetine. The concentrations of fluoxetine in hair and urine extracts were 40.9 ng/mg and 10.8 ng/mL, respectively; the concentrations of norfluoxetine were 4.94 ng/mg and 7.57 ng/mL, respectively. Conclusion A method for the determination of fluoxetine and norfluoxetine in human hair and urine by GC-MS/MS was developed and applied to real cases. Furthermore, the chemical modification effects of five derivatization reagents on fluoxetine and norfluoxetine were compared, and the best effect was obtained by HFBA at 70 °C for 45 min.
研究领域:
分析化学
·
毒理学
·
临床医学
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高影响因子
Foods
·
2021
·Vol. 10
·期 11
·2735
·
IF 4.35
Chujun Liu,Yawen Guo,Bo Wang,Lan Chen,Kaizhou Xie,Chenggen Yang
A simple and sensitive gas chromatography–tandem mass spectrometry (GC–MS/MS) method was established for the quantitative screening of penicillin G residues in chicken and duck eggs (whole egg, yolk and albumen). The analyte was separated on a TG-1MS capillary column (30.0 m × 0.25 mm i.d., 0.25 μm) with an external calibration method and electron impact (EI) ionization. Samples were pretreated using an accelerated solvent extraction (ASE) procedure followed by solid-phase extraction (SPE) on HLB cartridges (60 mg/3 mL). The derivative, which was safer and easier to store than penicillin G, was obtained by reacting trimethylsilyl diazomethane (TMSD) with penicillin G. The method was validated by the following parameters: linearity, accuracy, precision, limit of detection (LOD) and limit of quantification (LOQ). The matrix-matched calibration curves had good linearity (R2 ≥ 0.9994) within the concentration range of LOQ–200.0 µg/kg for penicillin G in the sample matrices. In the same concentration range, the accuracy, in terms of recovery, was 80.31–94.50%; the relative standard deviation (RSD), intra-day RSD and inter-day RSD ranged from 1.24 to 3.44%, 2.13 to 4.82% and 2.74 to 6.13%, respectively. The LODs and LOQs of penicillin G in the matrices were in the ranges of 1.70–3.20 and 6.10–8.50 μg/kg, respectively. The applicability of the GC–MS/MS method was demonstrated by the determination of poultry eggs obtained from local markets with no penicillin G residues.Keywords:penicillin G;GC–MS/MS;ASE;poultry eggs;SPE
研究领域:
分析化学
·
食品安全
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PubMed
高影响因子
Separations
·
2023
·Vol. 10
·期 4
·231
·
IF 2.6
Chang-Seob Seo,Hyeun-Kyoo Shin
Gongjindan (GJD) is a traditional Korean medicine consisting of four herbal medicines and two animal-derived medicines, and is taken as a tonic in Republic of Korea. In this study, the goal was to develop and validate a simultaneous analytical method to quantify eight compounds in commercially available GJD samples using high-performance liquid chromatography (HPLC), ultra-performance liquid chromatography with tandem mass spectrometry (UPLC–MS/MS), and gas chromatography with tandem mass spectrometry (GC–MS/MS) systems. In HPLC and UPLC–MS/MS, seven components (gallic acid, 5-(hydroxymethyl)furfural, morroniside, loganin, nodakenin, decursin, and decursinol angelate) were separated and quantified using a distilled water–acetonitrile mobile phase system on a Capcell Pak UG80 C18column and an Acquity UPLC BEH C18 column, respectively. Muscone was quantified using GC–MS/MS. The developed assays were validated by evaluating the linearity, limit of detection, limit of quantitation, recovery, and precision. In the regression equations of all compounds, the coefficient of determination was ≥0.9917, showing good linearity. The recovery was 93.70–108.17%, and the relative standard deviation values in the precision test were all <1.50%. Using the developed analysis methods, GJD samples were determined to contain the eight target compounds in concentrations from non-detected to 10.75 mg/g. The analytical assays developed and validated in this study can be used to obtain data for the quality control of commercially available GJDs and for the further expansion of efficacy and clinical studies.
研究领域:
中药学
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分析化学
·
药理学
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高影响因子
ANALYTICAL LETTERS
·
2022
·
IF 2.267
Yimei Zeng,Changliang Ke,Qi Liu,Ke Huang
Organophosphate esters (OPEs) are commonly used in commercial products as flame retardants. In the present study, a simple method was established for the simultaneous determination of 10 OPEs in aquacultural water and sediments. The targets were extracted using dichloromethane or ethyl acetate, cleaned up by solid-phase extraction, and determined by gas chromatography – tandem mass spectrometry. The matrix effects were lower than 20% for all OPEs except for tris(2-chloroethyl) phosphate in sediments (matrix effect: 29.4%). In spiked water samples, the recoveries of the OPEs were from 72.3% to 108% with relative standard deviations ≤10.2% and the limits of detection from 0.17 to 1.13 ng·L−1. In spiked sediments, the recoveries of the OPEs were from 101% to 121% with relative standard deviations ≤11.2% with limits of detection from 0.02 to 0.32 ng·g−1, dry weight (dw). The developed method was applied to the analysis of aquaculture samples from Kaozhouyang Bay, China. The total concentration ranges of the 10 OPEs in the water and sediments were from 121 to 159 ng·L−1 and 7.54 to 13.3 ng·g−1, dw, respectively.
研究领域:
环境科学
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分析化学
·
水质
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环境监测
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高影响因子
BIOMEDICAL CHROMATOGRAPHY
·
2021
·Vol. 35
·期 12
·e5209
·
IF 1.902
Yunheng Yao,Longlv Bai,Haifeng Tian,Xinzi Wu,Nianjie Zhang,Lunpeng Wu,Yifan Jia,Xiuli Ren
In this study, a new fluorinated methacrylamide (MACF) was synthesized and evaluated as an adsorbent in the dispersive solid-phase extraction for the effective determination and extraction of 20 organophosphorus pesticides (OPPs) from ginseng samples using the QuEChERS (quick, easy, cheap, effective, rugged, safe) method coupled with GC–MS/MS. The properties of MACF were characterized using Fourier-transform infrared spectroscopy, elemental analysis, and high-resolution 19 F NMR. MACF, chitosan, primary and secondary amine, octadecylsilane, graphitized carbon black, Z-Sep, Z-Sep + , and EMR-Lipid were compared in terms of extraction efficiency. The best results were obtained when MACF was used. Matrix-matched calibration was employed for quantification. All the OPPs exhibited good linearity ( r 2 > 0.9969) with the concentration at their respective concentration ranges. The limits of detection were 1.5–3.0 μg/kg, and the limits of quantification were 5.0–10.0 μg/kg. The trueness of the 20 pesticides at four spiked levels ranged from 86.1 to 111.1%, and the relative standard deviation was less than 11.3%. The modified QuEChERS method using MACF as the adsorbent was sensitive, reliable, and cost-effective and could be used for the determination of 20 OPP residues in ginseng.
研究领域:
分析化学
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环境科学
·
药学
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食品科学
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PubMed
高影响因子
JOURNAL OF CHROMATOGRAPHY B-ANALYTICAL TECHNOLOGIES IN THE BIOMEDICAL AND LIFE SCIENCES
·
2018
·
IF 2.441
Xiaoyu Lu,Min Fang,Yu Dai,Yue Yang,Ali Fan,Jiaqiu Xu,Zhiying Qin,Yang Lu,Di Zhao,Xijing Chen,Ning Li
PEGylation techniques have been increasingly employed in drug delivery system and chemical modification of compounds with low aqueous solubility. Triacontanol (TA) is a natural product with several pharmacological activities, but its low aqueous solubility significantly limited its application. PEGylated triacontanol (PEG-TA) was designed as the prodrug to improve the aqueous solubility and pharmacokinetic properties of TA. On the basis of salting-out assisted liquid-liquid extraction (SALLE) and saponification sample preparation procedure, a reliable gas chromatography tandem mass spectrometric (GC–MS/MS) method was developed and validated for the quantification of PEG-TA and its metabolite TA in rat plasma after separation and transformation. Acetonitrile-methanol (9:1, v/v) and ammonium acetate (10 M) were utilized to separate PEG-TA and TA (including conjugated TA with fatty acid). Saponification facilitated the complete conversion of PEG-TA into TA, so PEG-TA could be indirectly quantified. The results revealed that the GC–MS/MS method had excellent selectivity, accuracy and linearity. Calibration curves were linear (R 2 >0.99) within the range of 20.0–1000.0 ng/mL for TA and 100.0–10,000.0 ng/mL for PEG-TA. The intra- and inter-day precision of quality control samples were within 15%, and their accuracy values varied from 93.54% to 113.38%. This analytical method has been successfully applied to pharmacokinetic study of PEG-TA. This study can facilitate the further exploration and quantification of PEGylated prodrugs.
研究领域:
药物化学
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分析化学
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药理学
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高影响因子
JOURNAL OF CHROMATOGRAPHIC SCIENCE
·
2021
·Vol. 60
·期 2
·105-110
·
IF 1.618
Zhong ZhenHua,Chen YuPing,Xia HongYing,Chen ZhenZhen,Cheng QiZhen
A sensitive and selective gas chromatography–tandem mass spectrometry method was developed for the identification and quantification of five potential genotoxic impurities (PGIs), i.e., chloromethane, 2-chloropropane, 2-bromopropane, 4-chloro-1-butanol and diethyl sulfate, in abiraterone acetate. The method was validated according to the International Council for Harmonisation (ICH) guidelines. The linearity was established for the concentration range of 30–480 ng/mL (2-chloropropane, 2-bromopropane, 4-chloro-1-butanol and diethyl sulfate) and 90–1440 ng/mL (chloromethane). The correlation coefficient of each PGIs was >0.995. The extraction recoveries ranged from 90.49 to 106.79% for the five PGIs. The quantitation limit, detection limit, accuracy, precision, repeatability and stability of the method demonstrated that the method was an adequate quality control tool for quantitation and identification of chloromethane, 2-chloropropane, 2-bromopropane, 4-chloro-1-butanol and diethyl sulfate at trace levels in drug substances and drug products.
研究领域:
药物分析
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分析化学
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药品质量控制
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DOI
PubMed
高影响因子
ANALYTICAL LETTERS
·
2024
·
IF 1.6
Tongtong Liu,Weina Han,Lulu Wang,Xiaoyu Hou,Jin Cao
The aim of this study was to optimize the extraction conditions of 15 preservative allergens from skincare products using response surface methodology (RSM) and determination by gas chromatography – tandem mass spectrometry (GC-MS/MS). The optimal parameters were: 50% acetonitrile (ACN) (% v/v), a solvent/sample ratio of 80, and an extraction time of 10 min. The method provided good linearity (R2 ≥ 0.990) from 0.01 to 2 µg/mL with low limits of detection (0.02–0.2 mg/kg) and quantification (0.04–1 mg/kg). Recoveries ranged from 70.1 to 125.6% and the relative standard deviations (RSDs) varied from 2.0 to 14.9%. The method was successfully applied to eighty skincare products to accurately quantify these preservatives allergens.
研究领域:
分析化学
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化妆品科学
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DOI
高影响因子
JOURNAL OF CHROMATOGRAPHY A
·
2026
·
IF 4
Yehong Han,Juntao Wang,Weihua Liu,Pengfei Li,Meiting Zhang,Xuhui Jin,Zhi Wang
A low-cost, battery-free cold assisted SPME device with 40 min cooling was developed. • It demonstrated a higher extraction efficiency for volatiles than conventional SPME. • The efficient cooling enables 30%–44% improvement in PCNs extraction via CA-SPME. • The CA-SPME-GC–MS/MS method achieves enrichment up to 4299 for eight PCNs. • It was successfully applied to the determination of PCNs in drinking water samples. A cold-assisted headspace solid-phase microextraction (CA-HS-SPME) method combined with gas chromatography–mass spectrometry (GC–MS) was developed for the determination of eight polychlorinated naphthalene (PCN) congeners in water sample. In the CA-HS-SPME setup, frozen gel served as the refrigerant and copper tube as the thermal conductor to cool the polydimethylsiloxane (PDMS) fiber during extraction, thereby enhancing extraction efficiency. The main experimental variables affecting the extraction performance, including temperature, extraction time, and salt concentration, were systematically optimized. Under the optimized conditions, the method exhibited good linearity over the range of 0.1/0.5/1–500 pg/mL, with the correlation coefficient ( r ) values ≥ 0.9962. The enrichment factors for the PCNs ranged from 955 to 4299, while the limits of detection and quantification were 0.02–0.28 pg/mL and 0.07–0.92 pg/mL, respectively. The intra-day and inter-day precisions (n = 6), expressed as the relative standard deviations, were 10.8%–16.3% and 12.2%–17.8%, respectively. The recoveries obtained from fortified water samples ranged from 90.7% to 117.8%. The proposed method is sensitive, simple, solvent-free, and provides an effective approach for the determination of trace PCNs in water. Download: Download high-res image (169KB) Download: Download full-size image
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PubMed
高影响因子
Food Analytical Methods
·
2020
·Vol. 13
·期 3
·823-832
·
IF 2.667
Ye Xuemin,Shao Hua,Zhou Ting,Xu Jiahui,Cao Xiaoji,Mo Weimin
A modified QuEChERS protocol with a nitrogen-doped graphitized carbon derived from dicyandiamide sludge as a cleanup sorbent has been developed to determine 20 organochlorine pesticides in tomatoes using gas chromatography coupled to a triple-quadrupole mass analyzer. Compared with traditional QuEChERS adsorbents, N-doped graphitized carbon exhibited higher recoveries toward the target pesticides in tomatoes. And the modified protocol exhibited the advantages of environmental-friendly and low-cost. The use of dicyandiamide sludge to produce NGB as an adsorbent for QuEChERS opened up a new field for the comprehensive utilization of dicyandiamide waste. Under the optimum conditions, the modified method provided excellent linearity with correlation coefficient higher than 0.9980 and low limits of detection ranging from 0.001 to 0.1 μg/kg. The mean recoveries of the majority of pesticides in tomatoes ranged from 71.2 to 95.3% with relative standard deviation lower than 20%. Thus, the proposed protocol could be considered a good alternative for traditional QuEChERS method for pesticide analysis in agricultural vegetables.
研究领域:
食品科学
·
环境科学
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DOI
高影响因子
Foods
·
2025
·Vol. 14
·期 18
·3223
·
IF 5.1
Xianxiu Zhou,Jiajing Hu,Hongchun Cui,Jiahao Tang,Yongwen Jiang,Haibo Yuan,Jiahua Li,Yanqin Yang
Floral–fruity aroma Pu-erh tea (FFAPET) is highly valued by consumers for its distinctive and appealing fragrance. This study conducted a comprehensive investigation into the volatile components of FFAPET using advanced analytical techniques, including GC-O-MS, GC-MS/MS, aroma recombination, and omission tests. Compared with traditional stale aroma Pu-erh tea, FFAPET exhibited higher levels of alcohols and alkenes. Through GC-O-MS combined with OAV analysis, 10 key active-aroma compounds were identified in representative FFAPET samples. These compounds included (E, E)-2,4-heptadienal, phenylethyl alcohol, geraniol, (E,Z)-2,6-nonadienal, (Z)-4-heptenal, 2-phenethyl acetate, 2,2,6-trimethylcyclohexanone,D-limonene,β-ionone, and linalool, all of which made significant contributions to the development of the characteristic floral–fruity aroma profile. Tests involving aroma recombination and omission further confirmed that seven of these odorants played essential roles in defining the overall aroma of FFAPET. These findings offer valuable theoretical insights for the enhancement and regulation of Pu-erh tea flavor, particularly for the optimization of the floral–fruity aroma characteristics.
研究领域:
食品化学
·
风味科学
·
分析化学
·
茶叶科学
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DOI
PubMed
高影响因子
Food Chemistry-X
·
2026
·
IF 8.2
Jingjing Yu,Yuxin Liu,Cong Wang,Mantang Chen,Cong Nie,Wei Liu
A deep eutectic solvents-based ferrofluids (DES-FFs) material was prepared by combining small-sized Fe 3 O 4 magnetic cores with a ternary choline chloride/sesamol/coumarin (1:3:1) DESs. The material was used for single-step magnetic-assisted liquid-liquid microextraction (MALLME) and determination of 15 pyrethroids (PYs) in vegetable oils by GC–MS/MS. The small-sized Fe 3 O 4 material improved colloidal stability of DES-FFs and enabled rapid phase separation (<10 s). The DES-FFs might leverage enhanced π-π stacking interactions between sesamol/coumarin and PYs, and optimal hydrophilicity-polarity matching, which collectively contributed to the high extraction efficiency for PYs. Comprehensive characterization (HRTEM, XRD, FTIR, TGA, etc.) validated the material's structural integrity, thermal stability and magnetic property. The developed method demonstrated high sensitivity (LODs: 0.91–3.03 ng/mL; LOQs: 3.02–10.09 ng/mL), significantly reduced matrix effect, and good precision (RSD ≤6.92%) for 15 PYs in vegetable oils, with recoveries ranging from 79.88% to 107.90%. Determination of 15 PYs was successfully achieved in both refined and crude vegetable oils.
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高影响因子
危险品化学品经营许可证（带存储）