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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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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DOI
PubMed
高影响因子
ANALYTICAL AND BIOANALYTICAL CHEMISTRY
·
2018
·Vol. 410
·期 15
·3587-3595
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IF 3.307
Chen Guilin,Wu Jianlin,Li Na,Guo Mingquan
Rhamnus davurica Pall. ( R. davurica ) has been used as a traditional medicine for many years in China and abroad and shown a wide spectrum of biological activities. Previously, we reported the phytochemical fingerprinting profile of R. davurica , its distinct anti-proliferative activities against HT-29 and SGC-7901 cell lines, and the topoisomerase I (Top I) ligands based on bio-affinity ultrafiltration and HPLC-MS (UF-HPLC-MS). Nevertheless, among the 32 peaks detected in the fingerprinting profile, the common bioactive constituents responsible for the anti-inflammatory and anti-proliferative activities in the extracts remain elusive. To further explore the specific responsible components for their diversified activities and their potential action targets/mechanisms, the method based on bio-affinity UF-HPLC-MS using therapeutic targets like Top I and cyclooxygenase 2 (COX-2) was established to rapidly screen and identify the ligands binding to these known target enzymes. As a result, 12 components were revealed as potential Top I ligands along with 11 components as potential COX-2 ligands, where several components were revealed to possess both activities. Further validations of these bioactive components have also been conducted and confirmed their highlighted activities. This integrated method of UF-HPLC-MS exhibits high efficiency in rapidly screening for multi-target bioactive components responsible for multiple pharmacological effects from the complex natural products and could be very useful to explain the complex action mechanisms of herb medicines in a complex multi-component and multi-target mode at the molecular level.
Schematic diagram of UF-HPLC-MS assay to screen for Top I and COX-2 ligands. The principle of the assay usually involves the following steps: incubation, ultrafiltration, and identification.
研究领域:
药理学
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植物化学
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分子生物学
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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
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产品关联
DOI
PubMed
高影响因子
JOURNAL OF CHROMATOGRAPHY A
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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
INTERNATIONAL JOURNAL OF MOLECULAR SCIENCES
·
2018
·Vol. 19
·期 2
·443
·
IF 3.687
Mengsha Li,Rui Guo,Fei Yu,Xu Chen,Haiyan Zhao,Huixin Li,Jun Wu
Arthrobacter pascensZZ21 is a plant-beneficial, fluoranthene-degrading bacterial strain found in the rhizosphere. The production of the phytohormone indole-3-aectic acid (IAA) by ZZ21 is thought to contribute to its ability to promote plant growth and remediate fluoranthene-contaminated soil. Using genome-wide analysis combined with metabolomic and high-performance liquid chromatography-mass spectrometry (HPLC-MS) analyses, we characterized the potential IAA biosynthesis pathways inA. pascensZZ21. IAA production increased 4.5-fold in the presence of 200 mg·L−1tryptophan in the culture medium. The transcript levels ofprrandaldH, genes which were predicted to encode aldehyde dehydrogenases, were significantly upregulated in response to exogenous tryptophan. Additionally, metabolomic analysis identified the intermediates indole-3-acetamide (IAM), indole-3-pyruvic acid (IPyA), and the enzymatic reduction product of the latter, indole-3-lactic acid (ILA), among the metabolites of ZZ21, and subsequently also IAM, ILA, and indole-3-ethanol (TOL), which is the enzymatic reduction product of indole-3-acetaldehyde, by HPLC-MS. These results suggest that the tryptophan-dependent IAM and IPyA pathways function in ZZ21.Keywords:Arthrobacter;IAA biosynthesis pathway;genome-wide analysis;metabolomics;HPLC-MS
研究领域:
植物学
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微生物学
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环境科学
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DOI
PubMed
高影响因子
MICROCHEMICAL JOURNAL
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2023
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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
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DOI
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
Natural Products and Bioprospecting
·
2019
·Vol. 9
·期 3
·201-208
·
IF 0
Liu Qi,Chi Quan,Fan Ru-Ting,Tian Hui-Dong,Wang Xian
Abstract A sensitive and rapid high performance liquid chromatography–mass spectrometry (HPLC–MS) method was developed and validated for simultaneous quantification of ten steroid hormones, including estrogens, androgens, progesterones, and corticosteroids four classes of steroids. The following ten steroid hormones were analyzed: progesterone, 21-deoxycortisol, estrone, 4-androstenedione, testosterone, dihydro-testosterone, androstenone, dehydroepiandrosterone, corticosterone and cortisone. Stable deuterated isotopes were used as internal standards for quantification. Sample preparation with and without derivatization were performed after liquid–liquid extraction, and the corresponding results were compared according to sensitivity and selectivity. Hydroxylamine derivatization was found to improve the ionization efficiency of the analytes for electrospray ionization MS analysis. The gradient of mobile phase and experimental parameters for HPLC separation were optimized. The lower limits of quantification were in the range of 0.05–5 ng mL −1 with wide linear range for the ten steroid hormones. The intra-day precision < 11.1% and recovery of 84.5–120% with negligible matrix effect were achieved, where within the acceptance limits of the FDA guideline. Total HPLC–MS analysis time was 6 min. This method enables simultaneous quantification of steroids in human serum. It will be helpful for the serum steroid profiling in order to understand various endocrinology diseases. Graphical Abstract
研究领域:
医学
·
内分泌学
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分析化学
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产品关联
DOI
PubMed
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
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肿瘤学
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产品关联
DOI
PubMed
高影响因子
Journal of the Taiwan Institute of Chemical Engineers
·
2018
·
IF 3.849
Cheng Chen,Yijie Han,Jing Guo,Lixiang Zhou,Yeqing Lan
In this study, silica gel (SG) was utilized as an assistant to improve the degradation efficiency of p -nitrophenol (PNP) via persulfate (PS) activated with zero-valent zinc (Zn(0)). The effects of various parameters such as the dosages of SG, PS, Zn(0), and the initial pH on PNP degradation via Zn(0)/SG/PS were investigated through batch experiments. The results demonstrated that SG exhibited a strong synergistic role in the decomposition of PNP via Zn(0)-activated PS due to the dispersion and buffering character of SG. The degradation efficiency of PNP was strongly related to the dosage of SG, PS, or Zn(0). A low pH favored of the degradation of PNP. Nevertheless, PNP could be efficiently removed in a pH range of 3 to 9. The radicals of SO 4 •− and • OH were verified to be responsible for the oxidative degradation of PNP. Nevertheless, the contribution of SO 4 •− to the degradation of PNP was much larger than that of • OH. Based on the analyses of HPLC-MS data, it could be determined that C 6 H 7 NO, C 6 H 6 O 2 , and C 12 H 7 N 3 O 8 were the main intermediates generated from the degradation of PNP via Zn(0)/SG/PS. Furthermore, the possible mechanism and the degradation pathways of PNP via Zn(0)/SG/PS were proposed. PS activated with Zn(0) in the presence of SG could be concluded as a promising approach for the degradation of PNP in aqueous solution.
研究领域:
环境科学
·
化学工程
·
分析化学
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DOI
高影响因子
危险品化学品经营许可证（带存储）