Food Analytical Methods
·
2025
·
IF 3
Yuan Haiyue,Wang Jiafu,Fu Jiqiang,Wang Jishi,Zhang Yanwei,Geng Yue,Li Bei,He Zeying
A multiresidue method for simultaneously detecting 523 pesticides and metabolites in vegetables using ultra-high-performance liquid chromatography and gas chromatography coupled to tandem mass spectrometry (UHPLC-MS/MS and GC–MS/MS) was developed and rigorously validated for accuracy, precision, linearity, quantification limits, and matrix effects. The validated method was applied to analyze 300 vegetable samples from Shandong province, China, collected in 2023. Results showed the detection of 94 pesticides overall, with a detection rate of 31.67% and a 4.00% exceedance rate of maximum residue limits. Leafy vegetables exhibited the highest detection rate, and insecticides were commonly used in vegetable production. Thiamethoxam was the most frequently detected pesticide. Some banned and restricted pesticides were found at low levels. Celery, Chinese cabbage, tomato, cucumber, eggplant, sweet pepper, and spinach showed the highest frequency of multiple residues. In several rare cases, potential risks to adults and children were identified, highlighting the need for continuous monitoring of pesticide residues to ensure consumer safety.
研究领域:
食品科学
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环境科学
·
分析化学
✓ 已验证
产品关联
DOI
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
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药理学
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产品关联
DOI
高影响因子
JOURNAL OF THE SCIENCE OF FOOD AND AGRICULTURE
·
2020
·Vol. 101
·期 7
·2779-2787
·
IF 2.614
Wenbi Guan,Yingxin You,Jialing Li,Jiaying Hong,Haiying Wu,Yanna Rao
BACKGROUND Penicillic acid (PA) is produced by Aspergillus spp. and Penicillium spp., which are common postharvest and storage fungi of fruits. PA can be of concern for human health because of its toxicity and high fruit consumption by the population. However, no data on PA occurrence in various fruits have yet been reported. A quick, easy, cheap, effective, rugged and safe (QuEChERS) approach for PA determination in various fruits was developed and applied to explore PA incidence in fruits. RESULTS The modified QuEChERS procedure with extraction by ethyl acetate and purification by multi-walled carbon nanotubes (MWCNTs), primary secondary amine (PSA) and octadecyl silane (C18) was established to determine PA in various fruits by high-performance liquid chromatography–tandem mass spectrometry (HPLC-MS/MS). The average recoveries were 72.9–102.2% and relative standard deviations (RSDs) were 1.3–7.9%. A total of 161 fruits samples, including kiwi, apple, peach, grape and mandarin/orange, were collected in southern China. The incidence of PA in fruits was 14.9% and the levels of PA contamination were 0.200–0.596 μg kg −1 . Our results suggested that orange/mandarin, grape and kiwi were favorable matrices for Aspergillus spp. and Penicillium spp. to produce PA, rather than peach and apple. CONCLUSION To the best of our knowledge, this is the first report about PA contamination in various fruits in China. Our study emphasizes the necessity of the current established method, which could be used for continuous monitoring of PA and reducing the health risk to Chinese consumers. © 2020 Society of Chemical Industry
研究领域:
食品安全
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分析化学
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微生物学
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产品关联
DOI
PubMed
高影响因子
FOOD CHEMISTRY
·
2022
·
IF 9.231
Songyang Yao,Xuening Liu,Yao Fu,Shengyu Guan,Yunjie Liu,Laiqing Yan,Pingli He,Guoshi Liu
Since the global demanding of natural melatonin-enriched milk has been significantly increased in the populations of children and elder, the accurate and quick melatonin detection from milk is urgently required. Thus, the regular methods no longer satisfy this requirement. In the current study, we reported a novel method to extract melatonin from milk for liquid chromatography-tandem mass spectrometry melatonin detection. This novel method was to use cold methanol (-20℃) to precipitate proteins and fat in milk with one step to extract melatonin. Compared to the regular methods, it was devoid of procedures of sample drying, solid phase extraction and sample reconstitution. It could short the extraction time from the regularly 150 min to 60 min/per 24 milk samples. We believe that this novel method provides a possibility to detect large scale of milk samples in relatively short time with more efficiency and less cost compared to the regular method.
研究领域:
分析化学
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生物医学
✓ 已验证
产品关联
DOI
PubMed
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
✓ 已验证
产品关联
DOI
PubMed
高影响因子
LWT-FOOD SCIENCE AND TECHNOLOGY
·
2016
·
IF 2.711
Xiaoqun Wei,Linzhou Zhuang,Chaomin Wu,Wenrui Chen,Zhiyong Li,Baojun Xu
A novel method for quantitative analysis of ethylenediaminotetracetic acid (EDTA) in wines and beers by liquid chromatography coupled to tandem mass spectrometry has been developed. Positive-ion mode was applied as the scan mode, amine species were firstly used as the derivatization reagents of EDTA, and phenylboronic acid was used to react with maltose to eliminate its matrix interference. Primary amines could efficiently eliminate the interference from metal ions (Fe(III) and Cu(II)). The responsive intensity of EDTA with amine derivatization could be improved over 300 times than that without adding amine species. The recovery rate was significantly increased to 104.1% after adding phenylboronic acid at 20.0 mg/L as compared to the control spike-and-recovery experiment results (1.3–1.7%) of beer samples without adding phenylboronic acid. The validated method showed excellent detection sensitivity (0.001 mg/L for LOD (limit of detection) and 0.004 mg/L for LOQ (limit of quantification)) with satisfactory recovery rates (76.0%–97.2%), and good precision (1.40–5.40% RSD values). The optimized method has been satisfactorily applied to the analysis of actual wine and beer samples. It can be proposed as a powerful analytical method of EDTA in wines and beers, and can even be adapted to detect other chelates and polydentate compounds.
研究领域:
分析化学
·
食品科学
✓ 已验证
DOI
高影响因子
JOURNAL OF FOOD COMPOSITION AND ANALYSIS
·
2024
·
IF 4
Zuolong Yu,Beizhen Hu,Yao Chen,Chaoqun Huang,Chao Han,Yan Shen
A gas chromatography-tandem mass spectrometry (GC − MS/MS) method was established for accurately determining penicillic acid in cereals. The cereal samples were extracted using acidified acetonitrile, purified by solid-phase extraction, and derived using N,O-bis(trimethylsilyl) acetamide for GC − MS/MS analysis. Recovery experiments were conducted with low, medium, and high concentrations. The recovery rates were 72.1%–89.8%, the relative standard deviations were less than 8.6%, and the limit of quantification was 20 μg/kg. The established method was rapid, efficient, sensitive, and specific, meeting the requirements for the determination of penicillic acid in cereals. The method exhibits high sensitivity, accurate results, and stable recovery, making it suitable for detecting penicillic acid residues in cereals.
研究领域:
食品科学
·
分析化学
✓ 已验证
产品关联
DOI
高影响因子
Journal of Forensic and Legal Medicine
·
2024
·
IF 1.2
Zhonghao Yu,Yuhao Yuan,Qing Shi,Hang Gao,Erjuan Zhao,Jinghong Ma,Yiwu Zhou
Brodifacoum, a long-acting anticoagulant rodenticide, exerts inhibitory effects on blood coagulation factor synthesis, leading to abnormal clotting function and potential fatality. Poisoning of accidental exposure to brodifacoum is not rare, but death from brodifacoum poisoning can be largely avoided with timely and long-term effective treatments, consequently, forensic data on fatalities due to brodifacoum poisoning may be limited. This paper presents a case of brodifacoum-induced homicide, detailing the medial records and pathological changes observed in multiple organs. Furthermore, t liquid chromatography–tandem mass spectrometry (LC-MS/MS) was employed to measure the concentrations of brodifacoum in blood, hydropericardium, and urine 40 days post-poisoning (1 day post-mortem), yielding values of 0.097 μg/mL, 0.089 μg/mL, and 0.007 μg/mL respectively. The aim of this article is to contribute towards forensic identification of fatalities resulting from brodifacoum poisoning while also serving as a reference for clinical diagnosis in similar cases.
研究领域:
法医学
·
毒理学
✓ 已验证
产品关联
DOI
PubMed
高影响因子
ANALYTICAL CHEMISTRY
·
2020
·
IF 6.785
Xue Zhao,Gang Wu,Wenpeng Zhang,Mengqiu Dong,Yu Xia
Sphingomyelins (SMs) are an essential class of lipids widely existing in different organisms. The sphingoid base and N-acyl chain are two building blocks which can undergo different types of modifications during lipogenesis, including desaturation, hydroxylation, and methyl branching. Current lipidomic analysis methods cannot provide detailed information on these structural motifs. Herein, we developed a tandem mass spectrometric method by harnessing radical-directed dissociation (RDD) from collision-induced dissociation (CID) of the bicarbonate anion adduct of SM ([M + HCO3]−). A major RDD channel produced a high-abundance fragment carrying the intact N-acyl chain, termed as “N-acyl fragment”, allowing the assignment of the sphingoid base/N-acyl composition and relative quantitation of compositional isomers of SM at high sensitivity. RDD also produced intrachain fragments in lower abundances, which helped localization of methyl branching and hydroxylation in SM. The acetone Paternò–Büchi (PB) reaction was found to be capable of derivatizing the Δ4 carbon–carbon double bond (C═C) in sphingosine (SPH) base and producing C═C diagnostic ions upon CID, albeit at much lower efficiencies than those of the isolated C═C in alkyl chains. A liquid chromatography–mass spectrometry workflow was developed by incorporating MS2 CID of SM via [M + HCO3]− and PB-MS2 CID. The capability of profiling SM with detailed structural information was demonstrated by analyzing complex lipid extracts from porcine brain and Caenorhabditis elegans. These results provided visualization of the sphingoid base/N-acyl compositional isomers of SM lipids and revealed large structural diversity from each sample. These included identification of the sphingadiene base [d18:1(Δ4,14)], C═C location isomers in N-acyls, C-2 hydroxylation of N-acyls, and iso-methyl branched SPH base.
研究领域:
生物化学
·
脂质组学
·
分析化学
✓ 已验证
产品关联
DOI
PubMed
高影响因子
MICROCHEMICAL JOURNAL
·
2023
·
IF 4.8
Shu Wang,Bingliang Zhang
Nitrilotriacetic acid (NTA) and ethylenediaminetetraacetic acid (EDTA), as widely used chelating agents, have created many environmental issues and raised much attention regarding their environmental occurrence. However, the determination of NTA and EDTA in samples of complex solution chemistry remains challenging. Here, we proposed a simple and sensitive method based on liquid chromatography tandem mass spectrometry (LC-MS/MS) to determine NTA and EDTA from aqueous samples without an enrichment step. During the analysis, H + -cation exchange was used to efficiently eliminate interference from metal ions. The intensity of NTA and EDTA with trimethylsilyldiazomethane methylation could be improved hundreds of times that of the virgin samples. To maximize sensitivity, the sample pretreatment methods, the derivatization procedures and the LC-MS/MS conditions were systematically optimized. The validated method showed low limits of quantification (0.4 μg/L for NTA and 1.5 μg/L for EDTA), a wide linear response (up to several mg/L, R 2 > 0.998), and good intra- and inter-day precision (relative standard deviation ≤ 11%). The reliability of this method was successfully validated by analysis of authentic water samples collected from three WWTPs and one river with satisfactory recoveries (80–117%). It can be proposed as a powerful analytical method of NTA and EDTA in authentic water samples and could potentially be adapted to detect other chelates and polydentate compounds.
研究领域:
环境科学
·
分析化学
✓ 已验证
产品关联
DOI
高影响因子
FOOD CHEMISTRY
·
2023
·
IF 8.8
Jinlong Wu,Changwen Chen,Yong Li,Ke Cao,Xinwei Wang,Weichao Fang,Gengrui Zhu,Lirong Wang
The characterization of peach metabolites and carotenoids during canning and storage remains unclear. The present study identified 658 metabolites and 40 carotenoids in peach fruits throughout the canning and storage using ESI-MS/MS and APCI-MS/MS based metabolome approach. A total of 282 differentially accumulated metabolites were found, mainly including 78 phenolic acids, 74 lipids, 61 flavonoids. Five esterified carotenoids (rubixanthin palmitate, β-cryptoxanthin oleate, β-cryptoxanthin laurate, β-cryptoxanthin palmitate, and β-cryptoxanthin myristate) were the main peach carotenoids, with a proportion of approximately 90%, while free carotenoids accounted for 4.22–5.95% during the entire processing period. Moreover, the total carotenoid loss rates for canning and storage were 56.67% and 46.55%, respectively. Compared to the loss of free carotenoids, esterified carotenoids were more stable during storage, while canning led to a greater loss of esterified carotenoids. The results provided new insights into the maintenance of health-related phytochemicals from canning processes.
研究领域:
食品科学
·
代谢组学
·
农学
✓ 已验证
产品关联
DOI
PubMed
高影响因子
Forensic Toxicology
·
2017
·Vol. 35
·期 2
·275-283
·
IF 3.744
Minakata Kayoko,Yamagishi Itaru,Nozawa Hideki,Hasegawa Koutaro,Suzuki Masako,Gonmori Kunio,Suzuki Osamu,Watanabe Kanako
Human urine samples are easier to obtain than human blood samples due to noninvasiveness. The urine levels of synthetic cannabinoids (SCs) in unchanged forms, however, are usually much lower than their blood and tissue levels and cannot be detected in most cases. Therefore, in the present work a sensitive analytical method was devised for the determination of urine levels of six SCs in unchanged forms such as N -(1-amino-3-methy-1-oxobutan-2-yl)-1-pentyl-1 H -indazole-3-carboxamide (AB-PINACA), N -(1-amino-3-methy-1-oxobutan-2-yl)-1-(4-fluorobenzyl)-1 H -indazole-3-carboxamide (AB-FUBINACA), N -[(1 S )-1-(1-aminocarbonyl)-2-methyl-propyl]-1-(cyclohexylmethyl)-1 H -indazole-3-carboxamide (AB-CHMINACA), N -(1-amino-3,3-dimethyl-1-oxobutan-2-yl)-1-(cyclohexylmethyl)-1 H -indazole-3-carboxamide (MAB-CHMINACA), methyl-2-[1-(5-fluoropentyl)-1 H -indazole-3-carboxamido]-3-methylbutanoate (5F-AMB) and methyl-2-[1-(5-fluoropentyl)-1 H -indazole-3-carboxamido]-3,3-dimethylbutanoate (5F-ADB). These SCs were extracted from urine via liquid–liquid extraction. The identification and quantitation were performed by a relatively new type of an instrument for liquid chromatography–tandem mass spectrometry. The limits of detection were as low as 3–8 pg/mL, and the quantitation range was 10–1000 pg/mL using 400 μL of urine. The urine levels of AB-PINACA and AB-FUBINACA of victim 1 were 23 and 10 pg/mL, those of AB-CHMINACA and 5F-AMB of victim 2 were 239 and 19 pg/mL, and those of MAB-CHMINACA and 5F-ADB of victim 3 were 229 and 19 pg/mL, respectively. To our knowledge, this is the first report dealing with successful analysis of low levels of parent synthetic cannabinoids in authentic human urine specimens.
研究领域:
毒理学
·
药物代谢
·
法医学
·
分析化学
✓ 已验证
DOI
高影响因子
危险品化学品经营许可证（带存储）