ACS Omega
·
2023
·
IF 4.1
Yue Chen,Deliang Gao,Yueming Wu,Ling Wang,Weidi Fan,Yun Gao,Wenli Wang,Li Su,Beixing Li,Wei Mu,Weili Yu
Bupirimate is widely used as a highly active systemic fungicide. However, the frequent and heavy use of bupirimate has led to pesticide residues in crops that threaten human health and food safety. At present, there is limited research on the detection of ethirimol, which is the metabolite of bupirimate. This study established an ultrahigh-performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS) method to simultaneously detect bupirimate and ethirimol residues based on QuEChERS pretreatment. The average recoveries of bupirimate and ethirimol in cucumber were between 95.2 and 98.7%, respectively, with relative standard deviations (RSDs) of 0.92–5.54% at fortified levels of 0.01, 0.1, and 5 mg L–1. The established method was used to determine the residues in field trials in 12 regions of China, and the final residues of bupirimate were all less than the maximum residue limit (MRL). Since the risk quotient (RQ) of bupirimate and ethirimol in cucumber was less than 1.3%, the dietary risk assessment indicated that bupirimate and ethirimol had a low long-term dietary risk to the general population in China. This study provides effective guidance on the proper use of bupirimate in cucumber fields and a reference for establishing the MRL of bupirimate in China.
研究领域:
植物保护
·
食品安全
·
分析化学
✓ 已验证
产品关联
DOI
PubMed
高影响因子
FOOD CHEMISTRY
·
2021
·
IF 7.514
Xuehua Wang,Fang Chen,Lingjun Ma,Xiaojun Liao,Xiaosong Hu
High hydrostatic pressure (HHP) processing has become a commercial success in fruit and vegetable processing. Herein, the effects of HHP and high-temperature short-time (HTST) processing on metabolic profiling in tomato juice was evaluated by UPLC–MS/MS, HPLC, and GC–MS; a total of 425 metabolites, 14 carotenoids, and 56 volatile compounds were identified in tomato juice. HHP processing affects the composition of the juice less than HTST processing, considering 4 and 33 differential metabolites discriminated after HHP and HTST processing, respectively. The total lycopene and carotenoid contents in tomato juice increased after HHP processing, while the β-carotene and lycopene contents decreased after HTST processing. Further, more volatile compounds and higher contents of aldehydes that contribute to green aroma and lower contents of alcohols were observed after HHP and HTST processing, respectively. These findings provide a comprehensive understanding of the advantages of HHP processing on metabolite profiles in tomato juice.
研究领域:
食品科学
·
分析化学
·
营养学
✓ 已验证
产品关联
DOI
PubMed
高影响因子
JOURNAL OF CHROMATOGRAPHY B-ANALYTICAL TECHNOLOGIES IN THE BIOMEDICAL AND LIFE SCIENCES
·
2024
·
IF 2.8
Yunfeng Zhu,Fangkai Wang,Xin Wang,Ya Cheng,Xingyu Wang,Ali Fan,Jiawei Chang
Taletrectinib is a potent selective ROS and pan-NTRK tyrosine kinase inhibitor (TKI) and has been developed to treat non-small cell lung cancer (NSCLC). To facilitate pharmacokinetic and toxicokinetic studies of taletrectinib, we developed a procedure for ultra-high-performance liquid chromatography tandem mass spectrometry (UPLC-MS/MS) to detect the plasma level of taletrectinib in dogs. This assay procedure was validated in compliance with FDA guidance. The dog plasma samples were spiked with internal standard (IS), followed by protein precipitation, and analyzed using a Waters ACQUITY BEH C 18 column coupled to a Thermo triple quadrupole mass spectrometer. Separation was executed using the acetonitrile-0.1 % formic acid solution with gradient elution, at a flow rate of 0.4 mL/min. Taletrectinib and IS were monitored by multiple reaction monitoring (MRM) with m / z 406.2 > 349.2 and m / z 441.2 > 138.1, respectively. The procedure demonstrated excellent linearity with a correlation coefficient greater than 0.999 within the concentration range of 0.2–200 ng/mL. The inter- and intra-day accuracy ranged from −5.25 % to 5.26 %, and the precision was below 6.39 %. Acetonitrile-mediated protein precipitation showed high extraction efficiency and a recovery above 85 %. The procedure was then applied to quantify taletrectinib in beagle dog plasma after oral and intravenous doses and achieved success. The obtained pharmacokinetic parameters indicated high bioavailability of taletrectinib (>85 %) and extensive tissue distribution (>40 L/kg).
研究领域:
药理学
·
肿瘤学
·
分析化学
✓ 已验证
产品关联
DOI
PubMed
高影响因子
FOOD CHEMISTRY
·
2026
·
IF 10.4
Sumei Ru,Jiaxin Li,Yingshuang Lu,Yan Zhang,Junping Wang,Lu Dong,Shuo Wang
Developed UPLC-MS/MS for 8 free/cross-linked AGEs quantitation. • Achieved LODs 0.8–2.5 μg/L, surpassing prior reports. • Assessed AGEs in meat products, showing processing impacts. A universal ultra-performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS) method was developed for the simultaneous detection of eight free- or cross-linked advanced glycation end products (AGEs), including Nε-carboxymethyllysine, Nε-carboxyethyllysine, N δ -(5-hydro-5-methyl-4-imidazolon-2-yl)ornithine, glyoxal-derived hydroimidazolone, methylglyoxal lysine dimer, glyoxal lysine dimer, pyrraline and argpyrimidine. This method achieved the separation and quantification of the eight AGEs substances within 16 min. All analytes exhibited high correlation coefficients (R 2 > 0.999) within their respective linear ranges. Limits of detection and quantification in reconstituted solution were 0.8–2.5 and 2.5–5.5 μg/L, corresponding to 0.08–0.25 and 0.25–0.55 mg/kg in samples. Respectively. Method validation was performed using crispy fried pork as a blank matrix. The recovery rates ranged from 85.5% to 122.0%, with acceptable intra-day and inter-day precision. This method was successfully applied to the detection of AGEs in 30 different representative meat products, providing technical support for the research on the formation and control of AGEs.
✓ 已验证
DOI
高影响因子
JOURNAL OF CHROMATOGRAPHY B-ANALYTICAL TECHNOLOGIES IN THE BIOMEDICAL AND LIFE SCIENCES
·
2026
·
IF 2.5
Yu Miao,Ning Zhang,Guolei Zhang,Runyi Ye,Linrui Li,Hongyu Xue,Lei Yin,Meiyun Shi
Ultrafiltration with UPLC-MS/MS assay simultaneously quantifies free, protein-bound, total paclitaxel in biosamples. • PTX-Nab in vivo shows sustained release, lower systemic exposure, longer half-life, lung/spleen accumulation. • The primary excretion pathway of paclitaxel shifts from renal to hepatobiliary following albumin nanoparticle formulation. Paclitaxel (PTX) has poor water solubility. Traditional formulations requiring solubilizers can induce allergic reactions and disrupt pharmacokinetics. Albumin-bound PTX nanoparticles (PTX-Nab) provide a solvent-free nanodelivery system that enhances solubility and may enable receptor-mediated tumor targeting. Comprehensive studies comparing its systemic pharmacokinetics, particularly the dynamics of free versus total drug concentrations and excretion routes, are still lacking. This study established a sensitive ultra-performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS) method coupled with ultrafiltration to simultaneously quantify free, protein-bound, and total PTX in rats following intravenous administration of PTX-Nab and conventional PTX-injection. PTX-Nab profoundly altered the pharmacokinetic profile. Despite a double dose (10 mg/kg), it exhibited significantly lower dose-normalized initial concentration ( C 0 /Dose) and systemic exposure (AUC/Dose) along with a longer elimination half-life (t 1/2 ) than the injection group (5 mg/kg), indicating sustained drug release and prolonged circulation. Tissue distribution showed preferential accumulation of PTX-Nab in lung and spleen. Excretion studies showed a change in the primary excretion route. Unlike the renal-excreted conventional injection, PTX-Nab enhanced fecal excretion (56.14% versus 16.50%). These findings elucidate how the albumin carrier reshapes the in vivo fate of PTX through sustained release, tissue targeting, and clearance redirection, providing crucial pharmacokinetic evidence for its clinical application and future nanocarrier development.
✓ 已验证
DOI
高影响因子
Food Science & Nutrition
·
2026
·Vol. 14
·期 4
·e71593
·
IF 5
Diaodiao Yang,Jianwen Liu,Yang Song,Yajing Ma,Hongkang Zhu,Qingfeng Zhou,Maomao Zeng
Dietary exposure to both processing contaminants and natural toxins in fried foods poses a potential health risk, but analytical methods for their simultaneous monitoring are lacking. To address this gap, a rapid and efficient method based on QuEChERS extraction and UPLC–MS/MS detection was developed for the simultaneous determination of two β-carboline heterocyclic amines (harman and norharman) and seven mycotoxins (fumonisins B1, B2, B3 and aflatoxins B1, B2, G1, G2). The optimized extraction utilized a 30:20:50 (v/v/v) acetonitrile/methanol/water mixture. The method was rigorously validated, showing high sensitivity (LODs: 0.021–0.232 ng/g; LOQs: 0.100–0.587 ng/g), accuracy (recoveries: 80.4%–109.3%), and reliability. When applied to real samples, the method not only confirmed its practicality across different matrices but also revealed a critical finding: the co-occurrence of heterocyclic amines and mycotoxins, particularly in fried peanuts. This study provides an essential tool for integrated food safety surveillance and highlights the need for combined risk assessment of multiple contaminants.
✓ 已验证
DOI
PubMed
高影响因子
FOOD CHEMISTRY
·
2025
·
IF 9.8
Xu Xu,Shiping Zhao,Mengyang Nan,Lanrui Yang,Jia Lv,Ziling Zhang,Haitao Yang,Wushuai Duan,Baocheng Ji
Matrix adsorbents play a crucial role in the rapid multiresidue detection of pesticides by LC–MS/MS. Herein, we report the development of three functionalized melamine sponges for facile matrix adsorption for rapid analysis of 43 pesticides in five fruits. The matrix purification was optimized to enable rapid operation in seconds via simple soaking and squeezing, eliminating time-consuming centrifugation step commonly required in traditional QuEChERS protocols. Considering the removal efficiencies of pigments, proteins, carbohydrates, and lipids, the combined use of these three sponges yielded superior overall matrix purification performance. Good validation results were acquired for all monitored pesticides in terms of good linearities (coefficient of determination ≥0.993), satisfactory recoveries (70.9 %–118.7 %, 70.8 %–120.0 %, and 70.0 %–114.3 % at three spiked concentrations), and relatively low limits of detection (0.02–5 μg·kg −1 ) and limits of quantification (0.05–10 μg·kg −1 ). The functionalized melamine sponges demonstrated prospective application potentials for the rapid and accurate analysis of multiple pesticides in various fruits.
研究领域:
分析化学
·
食品安全
·
环境科学
·
农药残留分析
·
质谱分析
✓ 已验证
产品关联
DOI
PubMed
高影响因子
MICROCHEMICAL JOURNAL
·
2025
·
IF 5.1
Liwei Xu,Qiongxian Yan,Zhixuan Zhou,Anil Kumar Anal,Zhiliang Tan,Shaoxun Tang
Dipeptides have shown great potential in improving the production performance of livestock such as cattle, sheep and goats. The ruminal fluid, a complex matrix sample, is a good research object to investigate the healthy status of ruminants and to discover the biomarkers. A pre-column derivatization with dansyl chloride method was established for accurate quantification of 47 dipeptides by liquid chromatography (LC) triple quadrupole linear ion traps tandem mass spectrometry. An optimized LC gradient ensured the separation of Dns-dipeptides on Kinetic XB-C 18 column by the MRM mode. The ruminal fluid was treated with acetonitrile, and then directly derivatization with dansyl chloride under the optimized pretreatment conditions. The linear correlation coefficients were all above 0.99 in the linear range, the detection limits and the limits of quantitation of Dns-dipeptides ranged within 0.03–6.06 ng/mL and 0.09–20.0 ng/mL, respectively. The accuracy and precision were both less than 15.0 %. The average recovery rate of most analytes was between 80.0 % and 122.0 %. Most analytes were stable in 4 °C for three days. Twenty-five dipeptides were detected in the ruminal and abomasal fluid samples collected from the goats fed with corn and soybean-based diet (CS) or mulberry silage (MS) by the method developed. Dns-Gly-Pro, Dns-Gly-Val and Dns-Phe-Ala were the most abundant in the ruminal fluid, while concentrations of Dns-Phe-Ala, Dns-H-Tyr-Leu and Dns-Leu-Leu were the greatest in the abomasal fluid. Concentrations of five dipeptides, including Dns-Trp-Glu-OH, Dns-L-Ala-L-Leu, Dns-Leu-Leu, Dns-Tyr-Glu-OH and Dns-Val-Tyr, in the ruminal fluid of MS group were consistently decreased ( P < 0.05). However, Dns-H-Pro-Phe-OH level in the abomasal fluid of MS group was increased ( P < 0.05). The development of this quantitative detection method will greatly facilitate the understanding of the mechanism of dipeptides metabolism and circulation in the gut of livestock.
研究领域:
分析化学
·
动物营养学
·
代谢组学
·
反刍动物生理学
·
质谱分析
✓ 已验证
DOI
高影响因子
BIOCHEMICAL PHARMACOLOGY
·
2025
·
IF 5.6
Yuxin Shen,Ruibin Li,Lu Cao,Jun Wu,Haoxin Fu,Peiqi Wang,Ren-ai Xu,Ling Ji
Donafenib is a deuterated drug used as a first-line treatment for unresectable hepatocellular carcinoma (HCC). And efavirenz is an antiretroviral for human immunodeficiency virus (HIV) treatment. Due to the high prevalence of HCC in HIV patients, the combination of the two drugs is increasingly common. This study developed an ultra performance liquid chromatography tandem mass spectrometry (UPLC-MS/MS) assay for simultaneous quantitative determination of donafenib and its metabolite donafenib N-oxide, and assessed the impact of efavirenz on donafenib metabolism. In this bioanalytical method, good linearity ( r 2 = 0.99) was observed for donafenib (5–40,000 ng/mL) and donafenib N-oxide (2–400 ng/mL), with lower limit of quantification (LLOQ) of 5 ng/mL and 2 ng/mL, respectively. The precision (RSD%) and accuracy (RE%) of both compounds were less than ±15 %. In addition, the results of recovery, matrix effect, and stability were all in accordance with FDA guidelines. In vitro , efavirenz inhibited the metabolism of donafenib in rat liver microsomes (RLM) and human liver microsomes (HLM) with the half-maximum inhibitory concentration (IC 50 ) values of 5.87 μM and 39.14 μM, respectively, with no time-dependent inhibition (TDI). Moreover, the mechanism of inhibition was a mixture type in RLM. In vivo , the AUC (0-t) , AUC (0-∞) and C max of donafenib and donafenib N-oxide were significantly increased in the presence of efavirenz, which indicated that efavirenz increased the exposure of donafenib in rats. In short, this UPLC-MS/MS method was reliable for quantifying donafenib and its metabolite, and the findings suggested that efavirenz had an inhibitory effect on the metabolism of donafenib in vitro and in vivo .
研究领域:
药物代谢
·
分析化学
·
药理学
·
肿瘤学
·
抗病毒治疗
·
转化医学
✓ 已验证
产品关联
DOI
PubMed
高影响因子
ANALYST
·
2018
·Vol. 143
·期 23
·5744-5753
·
IF 3.864
Wei Yang,Xia Wu,Tingting Liu,Ting Wang,Xiaohong Hou
An attractive triazine-based conjugated microporous polymer (TCMP) was fabricated via the Friedel–Crafts reaction and magnetized by a simple reduction co-precipitation method for the first time. The morphology and textural properties of the as-synthesized materials were characterized by scanning electron microscopy, Fourier transform infrared spectroscopy, powder X-ray diffraction, N2 adsorption measurements, elemental analysis, and magnetic measurements. The resulting magnetic triazine-based conjugated microporous polymer (MTCMP) was introduced as an efficient adsorbent for vortex-assisted magnetic solid phase extraction (MSPE) coupled with ultra-high performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS) for the determination of trace 5-nitroimidazoles (5-NDZs) in environmental water samples. The TCMP has abundant delocalized π-electrons and N-containing triazine that can generate π-interactions, intermolecular hydrogen bonds, and electrostatic interactions with polar 5-NDZs. Extraction parameters affecting the recovery efficiency of five 5-NDZs (metronidazole, ronidazole, secnidazole, tinidazole, and ornidazole), including the amount of the adsorbent, the pH value of the sample, the salting-out effect, the adsorption and elution time, and types and volume of the elution solvents, were investigated. Under the optimal conditions, a wide linear range, acceptable recoveries (ranging from 82.62% to 110.9% with the relative standard deviation lower than 9.58%), and good reproducibility (relative standard deviations less than 8.81% for intra-day and inter-day precision) were obtained. The limits of detection for the five analytes were between 0.012 and 0.035 ng mL−1. The established method is rapid, has high sensitivity and accuracy, and has been successfully applied to the detection of 5-NDZs in real environmental water samples.
研究领域:
分析化学
·
环境科学
·
材料科学
✓ 已验证
DOI
PubMed
高影响因子
FOOD CONTROL
·
2021
·
IF 5.548
Zhiyong Zhao,Tingting Fan,Hengchao E,Yanmei Zhang,Xiaobei Li,Xianli Yang,Enjing Tian,Ailiang Chen,Xiaoyan Zhao,Changyan Zhou
Mushroom poisoning is becoming a serious food safety and public health issue due to its high morbidity and mortality in some parts of the world. Identifying mushroom toxins at an early stage of suspected intoxication is crucial for therapeutic decision making. Ibotenic acid, muscimol, 2-amino-4,5-hexadienoic acid and 2-amino-4-pentynoic acid are a group of amino group-containing mushroom toxins that can lead to hallucination and neurotoxicity on humans. However, there is no method established for simultaneous detection of the four toxins. In this present study, a new derivatization method was developed for the determination of these toxins in mushroom and urine samples by ultra-performance liquid chromatography tandem mass spectrometry (UPLC-MS/MS). After sample extraction the extract was directly derivatized by using 9-fluorenylmethyloxycarbonyl chloride and multiple factors affecting derivatization reaction were systematically optimized to enhance method sensitivity. Furthermore, liquid-liquid extraction with dichloromethane was employed for purification of the derivatized products. The method was fully validated for linearity, sensitivity, recovery and precision. Recoveries of four mushroom toxins were in the range of 85%–101% for urine and 82%–108% for mushroom. The limits of quantification were from 0.05 to 1 μg/L in urine and 1–20 μg/kg in mushroom. In addition, the developed method was successfully applied on mushroom samples treated by cooking and digesting with artificial gastric juice, demonstrating that vomitus as well as cooked mushroom and its soup can be used as the valuable materials for identifying mushroom poisoning caused by these four toxins.
研究领域:
毒理学
·
分析化学
·
食品科学
✓ 已验证
产品关联
DOI
高影响因子
MOLECULES
·
2022
·Vol. 27
·期 22
·7947
·
IF 4.927
Qingmei Sun,Yawen Hong,Zhaoxu Yang,Peixia He,Chao Chen,Jincheng Wang,Qinjie Weng
Pyrroloquinoline quinone (PQQ) is a powerful antioxidant coenzyme existing in diet, benefiting growth, development, cognition function, and the repair of damaged organs. However, a method for detecting PQQ in vivo was rarely described, limiting the research on the bioanalysis and metabolic properties of PQQ. In this study, a novel, simple, and efficient ultra-high performance liquid chromatography/tandem mass spectrometry (UPLC-MS/MS) method was developed and validated to quantify the concentration of PQQ in rat plasma. Detection through mass spectrometry was operated by multiple reaction monitoring (MRM) in negative electrospray ionization mode with ion transitionsm/z328.99→197.05 for PQQ andm/z280.04→195.04 for the internal standard. The calibration curves were linear up to 10,000 ng/mL, with a lower limit of quantitation of 10 ng/mL. Inter-run and intra-run precision ranged from 1.79% to 10.73% and accuracy ranged from −7.73% to 7.30%. The method was successfully applied to a toxicokinetic study in Sprague–Dawley rats after the oral administration of PQQ disodium salt at doses of 250 mg/kg, 500 mg/kg, and 1000 mg/kg. The toxicokinetic parameters were subsequently analyzed, which may provide valuable references for the toxicokinetic properties and safety evaluation of PQQ.Keywords:PQQ disodium salt;UPLC-MS/MS;toxicokinetic;rat plasma
研究领域:
分析化学
·
毒理学
·
药代动力学
✓ 已验证
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）