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JOURNAL OF FOOD COMPOSITION AND ANALYSIS · 2024 · IF 4

Rapid determination of eight biogenic amines in air-dried yak meat by QuEChERS combined with ultra-performance liquid chromatography-mass spectrometry

Han Xia,Hongyan Zhang,Zhehui Zhu,Kai xuan Tong,Qiaoying Chang,Hongyi Zhang,Chunlin Fan,Hui Chen

A method for the determination of eight biogenic amines (BAs) in air-dried yak meat was established using ultra-performance liquid chromatography–mass spectrometry (UPLC–MS/MS) without derivatization. The conditions of UPLC–MS/MS, pH, hydration volume, extraction solvent, extraction salt, and clean-up sorbent were optimized according to the characteristics of the BAs and the sample matrix. The samples were extracted with acetonitrile, the extract was purified using primary secondary amine (PSA) and C 18 . The BAs were determined using multiple reaction monitoring (MRM) within 5 min. The eight BAs exhibited good linearity, and the determination coefficient ( R 2 ) was greater than 0.997. The limits of detection (LODs) and the limits of quantification (LOQs) ranged from 0.40 to 2.50 μg/kg and from 1.25 to 7.50 μg/kg, respectively. The accuracy was between 80.3 % and 109.6 %, with relative standard deviations (RSDs) between 0.4–7.1 %. The method was applied in the detection of representative commercial samples of different processing techniques. In this method, the sample was pretreated free of derivatization and was simple, rapid, with minimum personal error, and high sensitivity. The method was assessed via GAPI and BAGI, verifying its environmental friendliness and applicability. It provides reliable methodological support for the determination of BAs in meat products.

CAS / MDL: 1336-21-6
研究领域: 食品科学 · 分析化学
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JOURNAL OF CHROMATOGRAPHY A · 2012 · IF 4.531

A novel derivatization approach for determination of ketamine in urine and plasma by gas chromatography–mass spectrometry

Kaoqi Lian,Pingping Zhang,Lingmei Niu,Siyuan Bi,Shipeng Liu,Lingling Jiang,Weijun Kang

A new method was developed for determination of ketamine (KT) in urine and plasma samples by derivatization and gas chromatography–mass spectrometry. In this article, KT was first derivatized with sodium nitrite to volatile N-nitrosamines under acidic condition. Then the derivative had been identified by the mass spectra. The derivatization conditions including the amount of hydrochloric acid, the amount of sodium nitrite, reaction temperature, reaction time and the extraction reagents were optimized. Calibration curves were linear in the range of 0.04–20   μg   mL −1 for KT, and the limit of detection (LOD) and limit of quantitation (LOQ) were 0.01   μg   mL −1 and 0.04   μg   mL −1 , respectively. The results of recovery indicated that the method had good precision and reproducibility. Compared with existing derivatization methods, this method provided a rapid, convenient, effective and low-cost way for gas chromatography method of KT quantification.

研究领域: 分析化学 · 医学检验
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iScience · 2025 · IF 4.1

Fact or Fiction: What's in your 15N2 and 15NH3 cylinders for sustainable ammonia and urea research?

Sanli Tang,Chengliang Mao,Guanshu Zhao,Jessica Ye,Wenqiang Qu,Lei Wu,Geoffrey Ozin

Attaining reliable performance indicators via 15 N-labelling is a daunting research endeavor for sustainable ammonia and urea synthesis processes, as currently obtained reaction rates and yields are often low. However, artefact and misinterpretation can be induced by ppm-level impurities in commercial 15 N 2 and 15 NH 3 cylinders, which are not well understood. Here, we report quantitative in-line gas chromatography mass spectrometry (GC-MS) analysis of impurities in commercial 15 N 2 and 15 NH 3 cylinders at ppm level, in conjunction with 1 H-NMR methods, exemplified by 808—16252 ppm of 14 N 15 N, 2472—4891 ppm 15 NH 3 , 3—319 ppm 14 NH 3 , 0—231 ppm of 14 NO 2 , 0—176 ppm 15 NO 2 , and 0—566 ppm 15 N 16 O impurities, some of which were not reported in cylinder certification nor previous studies. The collected results have formed recommended protocols applicable to all future 15 N labelling experiments intended to eliminate false positives.

CAS / MDL: 29817-79-6
研究领域: 化学工程 · 环境科学 · 分析化学
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CHEMICAL RESEARCH IN CHINESE UNIVERSITIES · 2013 ·Vol. 29 ·期 4 ·653-656 · IF 0.735

High efficient extraction of phthalates in aquatic products by a modified QuEChERS method

Wang Wen-wen,Gao Fu-kai,Li Gui-zhi,Liu Zhen-bo,Liu Yong-ming

A simple, environmentally friendly and high efficient extraction method was proposed for the determination of five phthalates in aquatic products by gas chromatography combined with mass spectrometry detector (GC-MS). When this method was adopted, samples were pretreated by modified QuEChERS(quick, easy, cheap, effective, rugged and safe) method. An environmentally friendly extractant(ethanol aqueous solution) replaced toxic acetonitrile for extracting phthalates in the protein-matrix samples. Fluorescence quenching spectra of bovine serum albumin(BSA) with phthalates show that there was a high-affinity interaction between phthalate and protein, decreasing the extraction efficiency of phthalates from fish samples. However, in the 80%(volume fraction, φ ) ethanol aqueous solution, a slow but full protein denaturation takes place, which would cause the unfolding of protein and the release of phthalates. Meanwhile, the fat-soluble impurities are extracted less in φ (ethanol) 80% aqueous solution than in either φ (ethanol) 100% or hydrophobic solvents in the liquid-liquid extraction procedure. Therefore the purification steps were greatly simplified. Overall recoveries were 81.77%–90.5% with limits of detection between 2.53 and 9.61 μg/L, and relative standard deviation values at 1.15%–4.85%. The proposed approach was satisfactorily applied to the determination of phthalates in real aquatic products, such as fish, shrimp and oyster.

研究领域: 分析化学 · 环境科学
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JOURNAL OF PHARMACEUTICAL AND BIOMEDICAL ANALYSIS · 2025 · IF 3.1

A preliminary study on estimation of postmortem submersion interval of rat cadavers in freshwater through polyamine analysis in tissues

Pei Zhang,Wei Xia,Yang Bai,Fuyuan Zhang,Yan Zhang,Wei Jiang,Huiya Yuan

The estimation of postmortem submersion interval (PMSI) has always been an important scientific issue to be addressed in drowning cases. Traditional methods, such as corpse temperature analysis and the assessment of corpse surface corruption, have limitations and cannot meet the need for accurate estimation of the time of death in the mid to late stages. Biogenic amines, as small molecules produced by protein degradation after death, have a certain regularity in relation to PMSI. To further explore the possibility of utilizing polyamines to estimate PMSI, this experiment constructed a rat cadaver model in both laboratory constant-temperature water and natural water bodies. Furthermore, cadaverine and putrescine in the liver and skeletal muscle were detected at different PMSI using gas chromatography-mass spectrometry (GC-MS). Through statistical analysis, we have constructed eight sets of mathematical models for polyamines-PMSI estimation, and determined the applicable time range through derivative analysis. After evaluation the models, the error rate in inferring PMSI using the fitted equations was less than 30 % within 242 h. The models established in this study could accurately infer PMSI in the mid to late stages of the postmortem period, providing a feasible approach for the drowning forensic issue.

CAS / MDL: 12125-02-9 124-09-4
研究领域: 法医学 · 生物化学
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Journal of Radiation Research and Applied Sciences · 2022 · IF 1.773

Extraction and GC-MS analysis of phenolic acids in rhizosphere soil of Pinellia ternate

Lifen Meng,Zhi Xia,Jingsong Lv,Gaofu Liu,Ye Tan,Qianzhu Li

In this paper, five phenolic acids in the rhizosphere soil of Pinellia ternate were determined to have strong allelopathy to Pinellia ternate . The phenolic acids in rhizosphere soil and non continuous cropping soil of Pinellia ternate for two years were extracted and detected by GC-MS, 5 phenolic acids were found to have different content changes. By comparing the contents of phenolic acids in the rhizosphere soil before, during and after planting, and combining with the literatures, it was determined that protocatechuic acid, vanillic acid, vanillin, syringate and syringaldehyde had strong allelopathy on the growth and development of Pinellia ternate . Furthermore, the effects of the above five phenolic acids on the growth of Pinellia ternate , the growth of seedlings and the comparison of tuber size were investigated. The results showed that the five phenolic acids had inhibitory effects on the growth of Pinellia ternate .

研究领域: 植物学 · 生态学 · 农学
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Analytical Methods · 2023 ·Vol. 16 ·期 1 ·114-121 · IF 3.1

Simultaneous determination of methyltestosterone and its metabolite in fish by gas chromatography-mass spectrometry

Liufeng Zhang,Juan Sun,Yinmeng Ding,Li Li,Jing Liu

Methyltestosterone is one of the banned drugs in aquaculture, and it should be monitored in food-producing animals. 17α-Methyl-5β-androstane-3α,17β-diol, as the main metabolite of methyltestosterone in vertebrates, could be used as another marker for controlling the administration of methyltestosterone, due to its high residual concentration and slow elimination rate. In this study, an analytical method based on gas chromatography-mass spectrometry (GC-MS) was developed and validated for the simultaneous determination of methyltestosterone and its main metabolite in fish. After pretreatment by liquid–liquid extraction with n-hexane and solid phase extraction with C18 and NH2 columns, the target analytes in the muscle tissues were extracted and concentrated, and the influence of the sample matrix was eliminated. Then, the prepared samples were separated and detected with GC-MS in the selected ion monitoring (SIM) mode. Methyltestosterone-D3 was chosen as the internal standard for quantitation. After optimization, the limits of detection for methyltestosterone and 17α-methyl-5β-androstane-3α,17β-diol were 20 μg kg−1 and 15 μg kg−1, respectively. The limits of quantitation were both 50 μg kg−1. The calibration curves showed good linearity in the concentration range from 50.0 ng mL−1 to 500.0 ng mL−1. The correlation coefficients of methyltestosterone and 17α-methyl-5β-androstane-3α,17β-diol were more than 0.9990. The recoveries of the analytes in real samples were in the range of 99.7–116.6% with the relative standard deviation of 5.2–8.3%. The established method could meet the demand for simultaneous detection of methyltestosterone and its major metabolite, and it could be used to provide more information on the abuse of methyltestosterone in food-producing animals.

CAS / MDL: 110-54-3 67-64-1
研究领域: 分析化学 · 水产养殖 · 食品安全
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CHEMOSPHERE · 2016 · IF 3.698

Simultaneously determination of bisphenol A and its alternatives in sediment by ultrasound-assisted and solid phase extractions followed by derivatization using GC-MS

Qiang Wang,Lingyan Zhu,Meng Chen,Xinxin Ma,Xiaolei Wang,Junchao Xia

Bisphenol analogues are a group of chemicals which are being widely applied in industrial and household products owing to regulations on bisphenol A (BPA) in many countries. In this study, an analytical method, including extraction from complex environmental matrices, clean-up using solid phase extraction (SPE) and following-up derivatization prior to gas chromatography coupled with mass spectrometry (GC-MS), was developed to analyze seven commonly used bisphenols in sediment. Five kinds of extraction solvents , four kinds of SPE cartridges, and four kinds of SPE eluting solvents were individually tested for their performances; and the conditions for derivatizing were also optimized. Finally, C 18 cartridge was determined as the SPE cartridge and methanol was selected as extracting and eluting solvent. Acetic anhydride (AA) was used as derivatizing agent and reaction took 20 min at room temperature. The method was used successfully to measure the seven bisphenol compounds in sediment samples from Taihu Lake, China. BPA, bisphenol F and bisphenol S were detected in all sediment samples, with concentrations in the range of 3.94–33.2; 0.503–3.28 and 0.323–27.3 ng g −1 dw. Other compounds were detected at low frequencies or not detected. We provided a convenient, reliable, and sensitive method to analyze bisphenol compounds in complex environmental samples.

研究领域: 环境科学 · 分析化学
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JOURNAL OF FOOD QUALITY · 2018 · IF 0.841

Survey of Octylphenol, Nonylphenol, and Bisphenol A in Infant Milk Powders by Solid-Phase Extraction Combined GC/MS Method

Chenggang Cai,Yibin Ying,Pinggu Wu,Jun Tang,Liyuan Wang,Tan Ying

A detection method for 3 kinds of phenolic compounds of endocrine disruptors (4-nonylphenol, 4-octylphenol, and bisphenol A) in infant milk powders by solid-phase extraction combined GC-MS was established. This method can effectively remove interference materials from infant milk powder products. The limit of detection and the limit of quantitation of the 3 kinds of compounds were 0.8 μg/kg and 2.5 μg/kg, respectively, with the relative standard deviations of 4.3–12.1%. The recovery rates of 4-nonylphenol, 4-octylphenol, and bisphenol A were of 68.5–89.2%, 64.8–87.0%, and 97.8–110.0%, respectively. Concentrations of the bisphenol A were from 0.8 to 14 μg/kg in 35 samples of the total 60 samples. And the other two compounds of 4-nonylphenol and 4-octylphenol were not found in all the 60 samples tested. The established method is simple, rapid, accurate, and highly sensitive, and the pollution of endocrine disruptors in some infant milk powders products was detectable in trace amounts.

研究领域: 分析化学 · 环境科学 · 食品科学
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RSC Advances · 2017 ·Vol. 7 ·期 85 ·53720-53727 · IF 3.108

Magnetic graphene solid-phase extraction in the determination of polycyclic aromatic hydrocarbons in water

Liling Pang,Wanfeng Zhang,Weiya Zhang,Pin Chen,Jing Yu,Gang-Tian Zhu,Shukui Zhu

In this work, magnetic graphene nanocomposite Fe3O4/rGO was fabricated by using a solvothermal method and applied to the magnetic solid-phase extraction (MSPE) of polycyclic aromatic hydrocarbons (PAHs) in environmental water samples, followed by gas chromatography-mass spectrometry (GC-MS). Several parameters affecting the extraction efficiency, such as amount of magnetic graphene, extraction time, desorption conditions, were studied in detail. The results showed that Fe3O4/rGO has an extremely high adsorption capacity for PAHs, only 10 mg of the adsorbent was needed for 100 mL of water sample, and the PAHs could be completely desorbed with 100 μL of desorption solvent. Under the optimized conditions, a good linearity was obtained in the concentration range of 0.005–5 μg L−1 for 10 low ring PAHs from naphthalene to chrysene, 0.1–5 μg L−1 for benzo[b]fluoranthene, benzo[k]fluoranthene and benzo(a)pyrene. The limits of detection (LOD, S/N = 3) of the method were in the range between 0.02–14.3 ng L−1. The recoveries for PAHs tested in spiked water samples were in the range 75.6–112.4% with relative standard deviations (RSD) ranging from 0.1–9.5%. Finally, the method was successfully applied for the analysis of real water samples in the search for PAHs.

CAS / MDL: 7782-42-5
研究领域: 环境科学 · 分析化学
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ANALYTICAL AND BIOANALYTICAL CHEMISTRY · 2019 ·Vol. 411 ·期 10 ·2209-2221 · IF 3.286

A double-functionalized polymeric ionic liquid used as solid-phase microextraction coating for efficient aromatic amine extraction and detection with gas chromatography–mass spectrometry

Zhang Yinchenxi,Duan Yixiang

A solid-phase microextraction (SPME) fiber based on a new polymeric ionic liquid was prepared for the extraction of trace aromatic amines in water and their detection by gas chromatography–mass spectrometry (GC–MS). The newly designed polymeric ionic liquid with two functional groups (benzene ring and ether group) was synthesized and fixed on stainless steel wire to effectively extract aromatic amines. Parameters that affect the extraction efficiency of the SPME fiber (extraction temperature, extraction time, alkali concentration, and salt concentration) were optimized to establish a headspace SPME–GC–MS method. The correlation coefficients were 0.996 or greater for concentration of the aromatic amines ranging from 0.01 to 10 μg mL -1 . In addition, the limits of detection for the new fiber are as low as 0.67 ng mL -1 , which is lower than that obtained with polyacrylate. The relative standard deviations of five consecutive extractions for the solution spiked at 1 μg mL -1 by the same fiber were all below 8.3%, and the interfiber relative standard deviations for the solution spiked at the same concentration ranged from 8.9% to 15.2%. Furthermore, long lifetime and good solvent resistance are exhibited by the fiber. Finally, satisfactory relative recovery in the range from 85.3% to 101.9 % was achieved for two environmental water samples.

研究领域: 分析化学 · 环境科学
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JOURNAL OF AOAC INTERNATIONAL · 2020 ·Vol. 104 ·期 3 ·712-718 · IF 1.51

Comprehensive Analysis of Volatile Compounds in Mouthpiece Cigarette Adhesive by Coupling Headspace with Gas Chromatography–Mass Spectrometry

Wei Min,Zheng Feng,Song Xuyan,Li Ran,Pan Xi,Guo Guoning,Yu Qiongwei,Feng Yuqi

BackgroundSome volatile compounds in mouthpiece cigarette adhesive emit irritating odors and affect the taste of smoking cigarettes. Therefore, it is necessary to monitor the volatile compounds in mouthpiece cigarette adhesive.ObjectivesA rapid and simple analytical method of volatile compounds in mouthpiece cigarette adhesive was established.MethodsIn this study, headspace (HS) injection coupled with GC–MS was utilized for qualitative and quantitative analysis. Initially, the volatile compounds in mouthpiece cigarette adhesives were detected by HS-GC–MS, followed by spectrum library retrieval. The detected compounds with the similarity to a spectrum library of more than 85% were further identified by comparing the retention time and mass spectra of the detected volatile compounds and those of the corresponding standard samples. The quantitative analysis of nine identified volatile compounds was performed.ResultsEleven volatile compounds in the mouthpiece cigarette adhesive were accurately identified. The quantitative analytical method of nine volatile compounds in mouthpiece cigarette adhesive was validated to have good linearities (R2 > 0.9932) within the range of 20–5000 ng/g. The detection limits of 9 compounds were within the range of 3.1–147.7 ng/g. The intra- and inter-day relative standard deviations were less than 19.8%. The recoveries of these 9 compounds spiked into mouthpiece cigarette adhesive were 68.1–108.3%.ConclusionsThe proposed method is rapid, simple, and accurate for qualitative and quantitative analysis of volatile compounds in the mouthpiece cigarette adhesive.HighlightsThe developed analytical method is expected to be used to monitor volatile compounds in various adhesives.

研究领域: 分析化学 · 烟草科学
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