Antibiotics-Basel
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2022
·Vol. 11
·期 10
·1427
·
IF 5.222
Hongli Ye,Siman Li,Yinfeng Xi,Yongfu Shi,Xiaorui Shang,Dongmei Huang
Antibiotic drug residues are crucial to ensure food safety and minimize risk to human health. Herein, a sensitive high-performance liquid chromatography–tandem mass spectrometry (HPLC–MS/MS) method was developed and validated for the determination of antibiotic residues (mainly amphenicols) consisting of chloramphenicol (CAP), thiamphenicol (TAP), florfenicol (FF), and florfenicol amine (FFA) in aquatic products. Amphenicols were well separated on a Kinetex F5 (100 mm × 3.0 mm, 2.6 µm) chromatographic column with the mobile phases of 1 mM ammonium acetate aqueous solution and methanol solution and measured after positive and negative electrospray ionizations using four internal standards. To our knowledge, it was the first time to report the good performance of F5 column and four internal standards for the determination of amphenicols. The established method featured a good linear relationship between chromatographic peak area ratios and the concentrations of amphenicols (R2> 0.992), a wide and low detection matrix-based range of 0.01–5 μg/L, a low detection limit of 0.01 μg/kg, etc. The spiked assays evidenced the accuracy and reliability of the developed method with the recoveries between 84.0 and 105%, the intraday relative standard deviations (RSDs) over the range of 0.769–13.7%, and the interday RSDs over the range of 0.582–13.3%. Finally, the proposed method was applied to investigate amphenicol residues in various aquatic products, including fish, shrimp, crab, shellfish, and other aquatic species.Keywords:antibiotics;amphenicols;detection;sensitivity;aquatic products;HPLC–MS/MS
研究领域:
食品安全
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分析化学
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环境科学
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DOI
PubMed
高影响因子
FOOD CHEMISTRY
·
2020
·
IF 6.306
Zhenlan Xu,Lingxiangyu Li,Yi Xu,Shanshan Wang,Xiaoxia Zhang,Tao Tang,Jianzhong Yu,Huiyu Zhao,Shenggan Wu,Chunrong Zhang,Xueping Zhao
Dendrobium officinale Kimura et Migo ( D. officinale ) is a dual-use plant with both botanical medicine and food applications, drawing increasing attentions. Pesticides are inevitably applied on D. officinale in commercial artificial-sheltered cultivation, yet little is known about pesticide residue levels in D. officinale . A modified high through-put QuEChERS method coupled with HPLC-MS/MS was developed and validated to detect 76 pesticides in D. officinale . Graphitized multi-wall carbon nanotubes (g-MWCNTs) was selected as the clean-up sorbent, showing relative weak affinity to triazole fungicide having planar structure in their molecular and low matrix effects of pesticides in D. officinale samples compared to MWCNTs and pesticarb. The validated method was applied to analyze pesticide residues in 86 real D. officinale samples collected from three main producing provinces. 43 different pesticides were detected with highest residue of 6.11 mg/kg for dimethomorph. Given possible health risks related to pesticide residues, accordingly, risk assessment of human exposure to pesticides via intake of D. officinale was thus performed, indicating that the pesticide residue in fresh or dry D. officinale would not cause potential risk to human health either in the long-term or short-term. This work improved our understanding of potential exposure risk of pesticide multi-residues in D. officinale .
研究领域:
药用植物学
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食品科学
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分析化学
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毒理学
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产品关联
DOI
PubMed
高影响因子
JOURNAL OF AGRICULTURAL AND FOOD CHEMISTRY
·
2022
·
IF 5.895
Siwei Wang,Xiaonan Wang,Hong Chang,Haibin Sun,Yanping Liu
The presence of pesticides in foodstuffs has received increasing amount of attention worldwide. In this study, an efficient and sensitive QuEChERS/HPLC-MS/MS-based method was established for the simultaneous detection of indaziflam, cyantraniliprole, spirotetramat, and their metabolites on fruits and vegetables. The purification procedure and detection condition parameters were optimized. Good precision and reproducibility were found for the method, and the average recoveries of the target analytes ranged from 71 to 118%, with the relative standard deviation ranging from 2 to 12%. The limits of quantification and the limits of detection were 1–5 and 0.3–1.5 μg kg–1, respectively. The proposed method was used to detect three pesticides and their metabolites in fruit and vegetable samples collected from China’s major producing regions. Furthermore, the dietary risk posed by the pesticide residues on fruits and vegetables was evaluated by risk quotients (RQs) and risk probabilities (RPs). The RQ and RP values were less than 100% for Chinese consumers. This study not only provides a reliable analytical method for monitoring purposes but also serves as a significant guide for food safety and export.
研究领域:
食品安全
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分析化学
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毒理学
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产品关联
DOI
PubMed
高影响因子
ENVIRONMENTAL SCIENCE AND POLLUTION RESEARCH
·
2023
·Vol. 30
·期 35
·84778-84790
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IF 5.8
Li Wei,Hou Huizhen,Hu Jiye
Consumers are becoming more concerned about pesticide residues in food. Since citrus represent a significant portion of the diet, it is appropriate to monitor the pesticide residues in citrus. In this paper, we modified a QuEChERS method combined with HPLC-MS/MS to investigate residue levels of 15 pesticides and 3 metabolites in citrus (whole fruit and pulp) and orange juice from the markets in China. And the dietary exposure risks were evaluated by using the hazard quotient (HQ) and hazard index (HI) methods based on deterministic and probabilistic models. The recoveries of the modified method ranged from 70 to 112% at three spike levels of 0.005–0.5 mg/kg with relative standard deviations of 1.0–18.1%. Pesticide residues were detected in 85.84% of the whole citrus and 40.00% of pulp, with concentrations ranging from 0.005 to 0.47 mg/kg, which did not exceed their maximum residue limits (MRLs) in China. The HQ (0.01–11.41%) and HI (0.07–16.2%) were both less than 100%, demonstrating that chronic, acute, and cumulative dietary risks were acceptable. Notably, the risk for children (1–6 years old, 1.96–16.2%) was higher than that for the general population (0.76–6.25%). The results of our study can provide a valuable reference for regular monitoring to protect public health and ensure pesticide management.
研究领域:
食品安全
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分析化学
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公共卫生
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产品关联
DOI
PubMed
高影响因子
JOURNAL OF CHROMATOGRAPHY A
·
2022
·
IF 4.601
Jiating Zheng,Xiaoru Peng,Taifeng Zhu,Shuyao Huang,Chao Chen,Guosheng Chen,Shuqin Liu,Gangfeng Ouyang
In recent years, bile acids (BAs), the important component of bile, were found closely related to the occurrence and development of diseases, therefore, determination of BAs in bile samples is of great significance. However, biological matrix complexity and low concentrations of BAs were still challenging for BA detection in small amount of bile samples. In this work, a core-shell NH 2 -MIL101@mSiO 2 was designed to improve the capture ability of BAs in biological samples, as well as possess good biocompatibility. Subsequently, solid-phase microextraction (SPME) probe of the NH 2 -MIL101@mSiO 2 was coupled with HPLC-MS/MS to establish the analysis method for detecting eight BAs in bile samples. The established method received extraction efficiencies of (30–2143)-fold higher than those of the commercial probes and low limit of detection (LOD ≤ 0.21 ng mL −1 ). The miniaturization of SPME sampling devices, as well as the low LOD of this work, endowed this method advantage of low consumption of bile samples (30 μL). Based on the proposed method, eight BAs in bile samples of pancreatic cancer patients and cholelithiasis patients were detected successfully. A distinct difference was found in the concentrations of four targeted BAs in bile samples from pancreatic cancer patients and cholelithiasis patients. This work provided a method for quantification of eight BAs in small volume human bile samples, and it could open up a perspective regarding the relationship between BA metabolism and the occurrence of diseases.
研究领域:
分析化学
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生物医学工程
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临床生化
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DOI
PubMed
高影响因子
BIOMEDICAL CHROMATOGRAPHY
·
2025
·Vol. 39
·期 5
·e70068
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IF 1.7
Sanwen Li,Qing Shao,Hongqun Qiao
Schisandrin B (Sch B), a natural lignan extracted from schisandra chinesis, has exhibited various pharmacological activities including anticancer effects. However, studies on the preclinical toxicokinetic profile of Sch B have not been publicly reported. This study aimed to investigate the preclinical concomitant toxicokinetics of multiple administration of Sch B. Sch B was administered orally to rats and dogs at 150, 300, and 600 mg/kg/day and 50, 100, and 200 mg/kg/day, respectively, for 26 weeks. Plasma concentrations of Sch B were determined by a validated HPLC–MS/MS method. According to the toxicokinetic results, significant gender differences were observed in the rats, and females had higher exposures than males for each dosing group. Toxicokinetic analysis demonstrated a notable accumulation in the plasma of dogs during the repeated administration of Sch B, and the degree of accumulation increased with the increase of the dose. The findings of this study indicated that there were differences in the concomitant toxicokinetics of Sch B between rats and dogs. These results can inform clinical studies and provide valuable insights for future human Sch B risk assessments.
研究领域:
药理学
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毒理学
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分析化学
✓ 已验证
产品关联
DOI
PubMed
高影响因子
JOURNAL OF CHROMATOGRAPHY A
·
2019
·
IF 3.858
Hui Chen,Chuanhui Huang,Wenming Zhang,Qingqing Ding,Jia Gao,Lan Zhang
An easy-prepared adsorbent with high stable and good dispersibility is especially valuable for the development of magnetic solid-phase extraction (MSPE) techniques. In this study, magnetic nitrogen-doped carbon nanotube cages (N-CNTCs) were synthesized via direct carbonization of cobalt (II)-containing metal-organic frameworks. During carbonization, cobalt ions inside the MOFs were converted into magnetic functional nanoparticles of N-CNTCs. Simultaneously, large amounts of nitrogen, originating from the organic ligands, were doped into the carbon framework. This unique structure gave the N-CNTCs excellent chemical stability, high affinity, and good dispersibility. The synthesized magnetic N-CNTCs were then used for MSPE of okadaic acid (OA) from aquatic samples. A simple, efficient, and sensitive method for detecting and quantitating OA was developed by combining the above sample pretreatment technique with high-performance liquid chromatography -tandem mass spectrometry (HPLC-MS/MS). The resulting method boasts a linear dynamic range of 3.0–1000.0 pg mL −1 with good linearity (R 2 ≥ 0.9994). The limit of detection (LOD) and limit of quantification (LOQ) were 1.3 pg mL −1 and 3.0 pg mL −1 , respectively. Several shellfish and seafood samples were analyzed using the developed method, showing satisfactory recoveries (82.0–107.0%) and relative standard deviations (<4.5%). The developed method was also used to investigate the OA distribution in crab tissues. Our results demonstrate that magnetic N-CNTCs are promising adsorbents for providing reliable support for the early warning and tracing to the source of algae toxins.
研究领域:
分析化学
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环境科学
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毒理学
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产品关联
DOI
PubMed
高影响因子
JOURNAL OF CHROMATOGRAPHY A
·
2022
·
IF 4.601
Shasha Zhang,Ran Wang,Yijing Wu,Zhuling Chen,Ping Tong,Yu He,Zian Lin,Zongwei Cai
Phthalate esters (PAEs) are a typical group of endocrine-disrupting chemicals (EDCs) and widely found in the environment, which have attracted great concern due to the potential risks to environment and human health. It is urgent to develop a high-efficiency and high-sensitivity analytical approach for enrichment and determination of ultra-trace PAEs. Herein, magnetic covalent organic frameworks (Fe 3 O 4 @TAPB-DVA) were fabricated via a one-pot approach at room temperature and explored as a magnetic enrichment probe with high surface area (275.50 m 2 /g), good crystallinity, regular pore size distribution (3.1 nm) and outstanding saturation magnetization (26.5 emu/g). Accordingly, a simple and sensitive method based on magnetic solid-phase extraction (MSPE) combined with HPLC-MS/MS was established to detect ultra-trace PAEs from fine particulate matter (PM 2.5 ) samples. The proposed method showed wide linear ranges (1-400 ng/L), good linearity (r > 0.9978) and high enrichment factors (EFs, 6.99-95.01 folds) with low detection limits (LODs) ranged from 0.01 to 0.5 ng/L (S/N ≥ 3). On this basis, the proposed method was substantially employed for sensitive detection of low- abundance PAEs from PM 2.5 samples, suggesting the promising application of the Fe 3 O 4 @TAPB-DVA in sample enrichment.
研究领域:
环境科学
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分析化学
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产品关联
DOI
PubMed
高影响因子
CHROMATOGRAPHIA
·
2025
·Vol. 88
·期 11
·891-903
·
IF 1.3
Li Wei-Si,Zhang Zhe-Meng,Wang Xue-Ying,Sun Chun-Xia,Liu Zhen,Ma Xiao,Qiao Zhou,Zhu Hai-Bin,Han Ling-Fei
Esomeprazole magnesium (EMO) is the S -enantiomer of omeprazole. As a second-generation proton pump inhibitor, it is more effective than omeprazole in inhibiting gastric acid secretion. Therefore, it is of great necessity to establish a quality control method to support its pharmaceutical development. The starting materials for the preparation of EMO may contain six potential genotoxic impurities (PGIs), designated as RC16, RC17, RC18, RC20, RC21, and RC23. These impurities have similar chemical structures, all containing benzene rings or pyridine rings with small differences in substituents, which leads to similar retention behaviors in the chromatographic column, and peak overlap is likely to occur during HPLC analysis, making it impossible to accurately determine the content of impurities. To enhance the quality control, this study established a sensitive and specific HPLC–MS/MS method. Utilizing electrospray ionization (ESI) in positive multiple reaction monitoring (MRM) mode, this method was used to determine the trace amounts of six PGIs in EMO raw material. On a 40 °C Inertsil ODS-SP C18 chromatographic column (4.6 × 150 mm, 5 μm), the six PGIs were well separated in an equilibrated elution mode at a flow rate of 0.5 mL min⁻ 1 . 0.5% formic acid in water and methanol were used as the mobile phase A and B, respectively. The method was rigorously validated in terms of precision, accuracy, limit of detection, limit of quantification, linear range, and robustness, and with all parameters meeting pre-defined acceptance criteria. Graphical
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DOI
高影响因子
MICROCHEMICAL JOURNAL
·
2023
·
IF 4.8
Jingjing Yu,Lili Shi,Yuxin Liu,Wei Liu,Mantang Chen,Xuehui Sun,Cong Nie,Fuwei Xie
FDA reported a HPHCs (Harmful and Potentially Harmful Constituents) list for tobacco products and tobacco smoke in 2012, which contained six carcinogenic aromatic amines (AAs). In this work, a sulfonated covalent triazine frameworks (CTF-SO 3 H) material was synthesized and used as a solid phase extraction (SPE) absorbent for highly effective enrichment and determination of six carcinogenic AAs in cigarette mainstream smoke (MSS), coupled with HPLC-MS/MS technique. The CTF-SO 3 H material was prepared with a rapid and facile method, which was superior to the general methods. The characterization with Nitrogen adsorption and desorption isotherm experiment, High resolution transmission electron microscopy (HTEM), etc, indicated that the CTF-SO 3 H material possessed sulfonic acid groups and abundant microporous structure. And the CTF-SO 3 H material showed good enrichment effect for AAs due to the synergistic effect of π-π stacking and electrostatic interactions. Limits of detection (LODs) of 6 AAs with the developed method were in the range of 0.01–0.11 ng cig −1 . Recoveries of 6 AAs were between 80.40% and 106.00%, while the intra-day and inter-day precisions were good (i.e. RSD intra ≤ 6.40%, RSD inter ≤ 9.90%). Commercial cigarette MSS samples were analyzed with the developed method, and a commercial cation exchange SPE column was chosen for comparison. Results obtained by two methods showed a good consistency. However, the CTF-SO 3 H material needed less dosage, even could be reused for 4 times. Thus, the developed method not only showed high enrichment efficiency, but also was economical.
研究领域:
分析化学
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环境科学
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毒理学
✓ 已验证
产品关联
DOI
高影响因子
JOURNAL OF PHARMACEUTICAL AND BIOMEDICAL ANALYSIS
·
2024
·
IF 3.1
Wenchan Deng,Rongrong Huang,Yuanjiang Pan,Cuirong Sun
The metabolism process of amino acids is closely related to the growth of normal and cancer cells. It is still not clear how L/D-configuration amino acids participate in the metabolism of colorectal cell. Herein, intra- and extra-cellular metabolic distribution of L/D-amino acids in colorectal cell (HCT116) and human normal intestinal epithelial cell (NCM460) were profiled utilizing HPLC-MS/MS coupled with a chiral probe. The results displayed the differential metabolic portrayal for the two cell lines. Compared with NCM460 cell, 13 kinds of significant differential amino acids were founded in a lower concentration within HCT116 cell, and L-Gln was even not detected for intra-cell; as for extra-cell culture medium, the HCT116 cell consumed more L-Gln, D-Phe and D-Leu, while L-Met was low ingested in HCT116 cell. L-Ala and Gly were excretion in both two cell lines, excepted L-Cit which was uptake in HCT116 and excretion in NCM460 cell. Furthermore, the dynamic changes of chiral amino acids displayed that phenylalanine, tyrosine and tryptophan biosynthesis and arginine biosynthesis is the major pathway for intra-cellular metabolites and extra-cellular metabolites, respectively. Moreover, with additional D-amino acids in culture medium, the results exhibited that high concentration of D-amino acids have no significant effect on the proliferation of NCM460 cell, but could influence the profiling of amino acids metabolites, and further affect the proliferation of HCT116 cell. This present work enhances the understanding of these differential amino acids metabolic network and depicts a dynamic process of metabolic dysregulation of HCT116 and NCM460 cell.
研究领域:
生物化学
·
肿瘤学
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产品关联
DOI
PubMed
高影响因子
FOOD CHEMISTRY
·
2021
·
IF 7.514
Hui Zhang,Guilin Chen,Yongli Zhang,Mei Yang,Jinming Chen,Mingquan Guo
Leaf of Nelumbo nucifera Gaertn. ( N. nucifera ) has been widely used as the main ingredient in lipid-lowering herbal teas and some prescriptions in China due to their excellent hypoglycemic and hypolipidemic effects. However, the active components responsible for these beneficial properties and their mechanisms remain unexplored. In this work, the N. nucifera leaf extracts significantly promoted the glucose consumption of HepG2 cells, and also exhibited remarkable inhibitory activities against α-glucosidase, pancreatic lipase, and COX-2. Furthermore, the top four potential active compounds ( N -nornuciferine, Nuciferine, 2-Hydroxy-1-methoxyaporphine, and Isorhamnetin 3-O-glucoside) targeting the above three enzymes were screened out by bioaffinity ultrafiltration with multiple targets coupled with HPLC-MS/MS. The enzyme inhibitory activities of candidate compounds were verified by enzyme inhibition assay and molecular docking. In addition, molecular docking revealed the binding information between the candidate molecules and enzymes. The current study provided valuable information in discovering functional active ingredients from complex medicinal plant extracts.
研究领域:
药理学
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生物化学
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药物化学
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产品关联
DOI
PubMed
高影响因子
危险品化学品经营许可证（带存储）