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
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毒理学
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药代动力学
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PubMed
高影响因子
JOURNAL OF THE SCIENCE OF FOOD AND AGRICULTURE
·
2023
·Vol. 103
·期 14
·6861-6870
·
IF 4.1
Feng Lan,Fudong Jiang,Hongwei Zang,Zhixin Wang
BACKGROUND Alternaria can infest pears to produce metabolites, which can contaminate pears and their processed products. Pear paste, one of the most important pear-based products, is popular among Chinese consumers especially for its cough relieving and phlegm removal properties. Although people are concerned about the risk of Alternaria toxins in many agro-foods and their products, little is known about the toxins in pear paste. RESULTS A method was developed for the determination of tenuazonic acid, alternariol, alternariol menomethyl ether, altenuene and tentoxin in pear paste by ultra-performance liquid chromatography tandem mass spectrometry with saturated sodium sulphate dissolution and acidified acetonitrile extraction. The mean recoveries of the five toxins were 75.3–113.8% with relative standard deviations of 2.8–12.2% at spiked levels of 1.0–100 μg kg −1 . Alternaria toxins were detected in 53 out of 76 samples, with a detection rate of 71.4%. Tenuazonic acid (67.1%), alternariol (35.5%), tentoxin (23.7%) and alternariol monomethyl ether (7.9%) were detected in all samples at concentrations of < limit of quantification (LOQ)–105.0 μg kg −1 , < LOQ–32.1 μg kg −1 , < LOQ–74.2 μg kg −1 and < LOQ–15.1 μg kg −1 , respectively. Altenuene was never found in pear paste samples. Tenuazonic acid, alternariol, tentoxin and alternariol menomethyl ether should be focused on due to their toxicity and detection rates. CONCLUSION To the best of our knowledge, this is the first report on the detection method and residue levels of Alternaria toxins in pear paste. The proposed method and research data can provide technical support for the Chinese government to continuously monitor and control Alternaria toxins in pear paste, especially tenuazonic acid. It can also provide a useful reference for related researchers. © 2023 Society of Chemical Industry.
研究领域:
食品安全
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分析化学
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植物病理学
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DOI
PubMed
高影响因子
JOURNAL OF AGRICULTURAL AND FOOD CHEMISTRY
·
2022
·
IF 5.895
Fanshan Feng,Wei Xiang,Han Gao,Yanan Jia,Yuansong Zhang,Lingshu Zeng,Jiaxin Chen,Xianzhi Huang,Li Xu
Mulberry twigs are an important source of α-glucosidase inhibitors. To date, research studies on α-glucosidase in mulberry twigs have mainly focused on alkaloids such as 1-deoxynojirimycin (DNJ). Preliminary studies have shown that there may be more active nonalkaloid α-glucosidase inhibitors in mulberry twigs. In this study, we immobilized α-glucosidase on Fe3O4@SiO2 for the first time and rapidly screened four nonalkaloid α-glucosidase inhibitors (kuwanon G, kuwanon C, kuwanon H, and morusin) using ligand fishing technology with ultrahigh-performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS) from the mulberry twig extract of Jialing 20, the excellent artificial triploid variety of mulberry cultivated extensively in Southwest China. The half maximal inhibitory concentrations (IC50) of kuwanon H and kuwanon G were 2.82 ± 0.68 and 2.83 ± 0.31 μM, respectively, with better inhibition activity than that of DNJ (with an IC50 of 7.04 ± 0.82 μM). Meanwhile, the molecular docking results showed that the action sites of these two isopentenyl flavonoids on α-glucosidase were different from that of DNJ. In brief, this work is beneficial to discovering new α-glucosidase inhibitors from mulberry twigs quickly and accurately and provides a theoretical basis for the mulberry twig extract as a functional food or a natural hypoglycemic drug source, as well as a reference for directional breeding of mulberry, which greatly improves the exploitation and utilization value of mulberry twigs as an agricultural byproduct in the fields of agricultural production, functional food, and natural medicine.
研究领域:
药理学
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分析化学
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天然产物
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农业科学
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功能食品
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产品关联
DOI
PubMed
高影响因子
BIOMEDICAL CHROMATOGRAPHY
·
2023
·
IF 1.8
Qiang Liu,Jin-Zhu Zhao,Fu-Sheng Zhou,Jiong Lan,Qiang Lu,Hong-Can Ren
GFH009 is a potent, highly selective, small molecule that targets and inhibits the activity of the CDK9/cyclin T1 regulatory complex of P-TEFb. This study aimed to develop and validate a highly selective and sensitive ultrahigh-performance liquid chromatography–tandem mass spectrometry (UHPLC–MS/MS) method for precise quantification of GFH009 in rat plasma. This method was subsequently employed for conducting toxicokinetic studies of GFH009 in rats. Plasma was prepared using a simple protein precipitation method by acetonitrile. Chromatographic separation of the analytes was achieved on a BEH C 18 analytical column with a rapid 3.0 min run time and a flow rate of 0.5 ml/min. The calibration curves for plasma samples exhibited excellent linearity over a wide concentration range of 1.0–1,000 ng/ml for GFH009. Intra- and inter-day accuracies were within 92.7–105.7%, and precisions were no more than 6.7%. Furthermore, the analyte demonstrated stability under four different storage conditions, with variations of <15.0%. This study pioneers a methodological innovation by introducing a highly reliable, specific and sensitive analytical method for GFH009 in rat plasma. The successful application of this method in toxicokinetic studies further underscores its significance, offering valuable insights for the methodology of clinical pharmacokinetic research.
研究领域:
药理学
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分析化学
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毒理学
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PubMed
高影响因子
CARBOHYDRATE POLYMERS
·
2024
·
IF 10.7
Ting Xue,Lei Zhou,Fanjun Wang,Zhuang Tian,Nanxi Li,Tong Ye,Ruolin Hao,Lei Yang,Ruolan Gu,Hui Gan,Zhuona Wu,Xiaoxia Zhu,Shuchen Liu,Yunbo Sun,Guifang Dou,Zhiyun Meng
In this study, a novel and accurate quantitative analysis method for the direct determination of chitosan (CS) in aqueous solutions using ultrahigh-performance liquid chromatography–tandem mass spectrometry (UPLC–MS/MS) is presented. By detecting the mass spectrum response intensity of a series of CS characteristic ion pairs , the sample concentration (abscissa) was linearly fitted with the total ion current (TIC) response intensity of its characteristic ion pairs (ordinate). A reliable standard curve was derived for quantifying CS in the range of 125–4000 ng/mL. Under the detection conditions, this CS quantification method yielded acceptable specificity (no interference peak), linearity (with correlation coefficient (r 2 ) values >0.999), precision (acceptable limit RSD r < 3 %, RSD R < 6 %), accuracy (RE within the acceptable limits of ±5 %), and stability (acceptable limit RE within ±5 %, RSD r < 3 %). Moreover, the applicability of measurement was verified when a series of substrates did not interact with CS in the solution. Results have verified the applicability of this method for determining CS content in different composites. This study provides a method for determining CS content with significant practical value and economic benefit.
研究领域:
分析化学
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药物分析
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生物技术
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DOI
PubMed
高影响因子
Food Chemistry-X
·
2023
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IF 6.1
Xinya Liu,Liqin Song,Baogui Xue,Zhuoheng Chi,Yuan Wang,Songqin Wen,Wenjuan Lv,Qiankun Hu,Qigao Guo,Shuming Wang,Di Wu,Guolu Liang,Danlong Jing
Triploid loquats are divided into yellow- and white-fleshed cultivars. To better understand taste variations in triploid loquat fruits, we used a UPLC-ESI-QTRAP-MS/MS-based widely targeted metabolomic analysis to examine the metabolic composition of two different color fleshed triploid loquats with a sample size of 54 and external validation method within a confidence level of P ＜0.05. We identified key flavor-related differentially accumulated metabolites using the variable importance in projection (VIP) value (VIP ≥ 1.0) and fold change ≥ 2 or ≤ 0.5. Furthermore, the results of the HPLC analysis showed that white-fleshed loquats had a low malic acid content. We also performed the UPLC-MS/MS system to investigate the carotenoids contents and lipidome in four triploid cultivars. In the fruits of white-fleshed varieties, the carotenoids contents were significantly downregulated, but the contents of most glycerolphospholipids were increased. Our results reveal the metabolomic changes between the yellow- and white-fleshed cultivars.
研究领域:
园艺学
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代谢组学
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植物生物化学
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产品关联
DOI
PubMed
高影响因子
BMC Pharmacology & Toxicology
·
2025
·Vol. 26
·期 1
·200
·
IF 2.7
Chen Xiaohai,Chen Dongxin,Wu Hualu,Xia Hailun,Lan Tian,Xu Ren-ai
This study aimed to develop and validate a novel ultra performance liquid chromatography tandem mass spectrometry (UPLC-MS/MS) method for the simultaneous determination of iloperidone (ILP) and its metabolites P88, P95 in rat plasma and to investigate drug-drug interaction (DDI) between shikonin and ILP in Sprague-Dawley rats. The separation of the analytes was performed on a UPLC BEH C18 column in the mobile phase (acetonitrile and water with 0.1% formic acid) with the flow rate of 0.4 mL/min. The quantitative analysis was performed in positive ion mode. A total of 10 Sprague-Dawley rats were divided into two groups: control group (1.0 mg/kg ILP alone) and experimental group (20 mg/kg shikonin plus 1.0 mg/kg ILP) to investigate the influence of shikonin on ILP metabolism in rats. We successfully established a quick UPLC-MS/MS analytical method for simultaneously detecting ILP and its two metabolites in rat plasma. Linearity, matrix effect, recovery, accuracy, precision and stability of this quantitative method was satisfied with Food and Drug Administration (FDA) guidelines. In addition, in vitro studies demonstrated that shikonin significantly inhibited CYP3A4- and CYP2D6-mediated metabolism in both rat liver microsomes (RLM) and human liver microsomes (HLM). Furthermore, we found the main pharmacokinetic parameters of ILP, such as AUC (0−t) and the peak plasma concentration (C max ), were obviously changed, which were about twice higher in experimental group than the values in control group. The data demonstrated that shikonin obviously changed the main pharmacokinetics of ILP and its metabolites in rats. In the future clinical use, we should pay more attention to the concomitant application of shikonin and ILP in humans.
研究领域:
药物分析
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药代动力学
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药物代谢
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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 CHROMATOGRAPHY A
·
2025
·
IF 4
Xu Xu,Shiping Zhao,Ziling Zhang,Lanrui Yang,Wenhao Zhao,Baocheng Ji,Yanhong Bai
In this study, a facile and efficient pipette tip-integrated silanized melamine sponge device was developed for the rapid quantification of multi-pesticide residues in cowpea by ultra-performance liquid chromatography-tandem mass spectrometry. By embedding silanized melamine sponges within a pipette tip architecture, the device facilitates efficient matrix cleanup through simple aspiration-dispensing maneuvers, substantially simplifying sample pretreatment workflows. Comparative evaluations against conventional commercial adsorbents revealed that the proposed system exhibits comparable or enhanced purification performance. Method validation demonstrated that target analytes achieved recoveries spanning 81.0%-115.4% across three spiking concentrations, with intra- and inter-day precisions both below 15%. Additionally, excellent linearity (R²≥0.9985), negligible matrix effects (-18.3% to 19.8%), and low limits of detection (0.025-2.40 μg·kg⁻¹) and quantification (0.05-5.00 μg·kg⁻¹) were attained. These findings underscore the considerable potential of the developed purification device for pesticide multi-residue analysis in complex food matrices.
研究领域:
分析化学
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食品安全
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环境监测
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农药分析
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产品关联
DOI
PubMed
高影响因子
JOURNAL OF CHROMATOGRAPHY A
·
2026
·
IF 4
Baocheng Ji,Yanxin Wang,Li Ma,Mengwei Zhang,Yumeng Liu,Xu Xu,Junguang Li,Ke Li,Dianbo Zhao,Yanhong Bai
A rapid, convenient, and efficient dispersive solid-phase extraction approach, integrating ultraperformance liquid chromatography–tandem mass spectrometry and pretreated pine pollen, was developed for sensitive quantification of 13 heterocyclic amines (HCAs) in sesame oil. Critical parameters, namely sorbent type and dosage, adsorption mode and duration, detergent dosage, eluent additive and volume, and elution cycles, were systematically optimized to evaluate their effects on the HCA recovery. The proposed method was verified for all the 13 HCAs, demonstrating favorable analytical characteristics with remarkable linear relationships (coefficient of determination, R 2 ≥ 0.998), adequate recoveries (64.2%–99.4%), acceptable intra- and inter-day precision (relative standard deviations ≤ 10.4%), and low limits of detection (0.02–0.83 μg/kg) and quantification (0.07–2.70 μg/kg). The proposed approach offers distinct advantages, including rapidity, simplicity, cost-effectiveness, and minimized organic solvent consumption, demonstrating great potential for accurately analyzing HCAs in complex food matrices.
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PubMed
高影响因子
JOURNAL OF CHROMATOGRAPHY A
·
2026
·
IF 4
Xiaoqian Wang,Yanhua Lai,Sufang Guo,Honglin Qin,Ziwang Liu,Ling Xia,Xuanjing Wang,Junzhang Wu,Gongke Li
In-syringe SPE-UPLC-MS/MS for profiling 43 Maillard reaction-related compounds. • Optimized conditions enable reliable retention of target analytes. • The developed method exhibited a wide linear range and low detection limits. • The developed method successfully applied to tobacco samples analysis. Considering the critical role of Maillard reaction-related compounds in determining the sensory and chemical stability of tobacco, this study develops an in-syringe SPE coupled with UPLC-MS/MS method for simultaneous determination of 43 Maillard reaction-related compounds in tobacco, covering reducing sugars (3), amino acids (17), Amadori compounds (17), and structurally related intermediates (6). The sample pretreatment utilizes HLB-packed self-assembled columns for SPE, followed by methanol elution. The extracted solution is then analyzed using a Titank C 18 column (150×2.1 mm, 1.8 μm), with acetonitrile and 0.1% formic acid aqueous solution employed as the mobile phase for gradient elution. Data were acquired in multiple reaction monitoring mode using electrospray ionization. Operation parameters were optimized systematically, including the type and amount of filler, solution pH, loading rate, elution solvent composition, and sample extraction volume. This method demonstrated excellent linearity for all 43 target compounds, with correlation coefficients exceeding 0.9980. The limit of detections was 0.10-0.50 µg/L for animo acids, 1.0×10 2 - 2.5×10 2 µg/L for reducing sugars, 0.10-5.0 µg/L for related Amadori compounds. This approach was successfully applied to the analysis of tobacco samples and extracts, providing a robust tool for studying the Maillard reaction and contributing to food safety assessment and optimization of food processing techniques.
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DOI
PubMed
高影响因子
MICROCHEMICAL JOURNAL
·
2025
·
IF 5.1
Wanxin Zhang,Yujie Chen,Zhe Song,Zhonghui Zhang,Bo Wu,Bin Di,Mengxiang Su
Synthetic cannabinoids (SCs) are new psychoactive substances with an increasingly large number of users and strong addictive properties. The metabolites produced after smoking SCs flow into sewage with urine and feces. Owing to the extremely low concentration of SCs and the complexity of sewage matrix, the development of different adsorbent materials to enrich SCs in sewage and enhance detection sensitivity is essential. However, existing adsorption materials, such as spherical magnetic solid-phase extraction (MSPE) materials, possess drawbacks of easily saturated functional sites, long extraction time, and low sensitivity. To solve these problems, we proposed two novel poly (glycerol methacrylate- co -trimethylolpropane trimethacrylate)/poly (dopamine- co -chitosan)-functionalized magnetic carboxylated multiwalled carbon nanotubes (GTMC/DCMC) as adsorbents and developed two highly sensitive quantitative analytical techniques to detect eleven SCs in wastewater. The magnetic adsorbents were fully characterized using transmission electron microscopy, infrared spectroscopy, vibrating sample magnetometry, and X-ray photoelectron spectroscopy. Additionally, two MSPE-UPLC-MS/MS methods were developed and validated to determine eleven trace analytes in wastewater. The validation results show that the limits of quantification (LOQ) of GTMC is 5.0 ng/L and the LOQ of DCMC is 2.5 ng/L. Additionally, the recoveries of GTMC range from 63.17 % to 86.22 %, and the recoveries of DCMC range from 61.29 % to 97.41 %. The relative standard deviations of intraday and interday precision are less than 10 %. The MSPE-UPLC-MS/MS methods are successfully applied to real wastewater samples, and the entire pretreatment process is completed in 25 min. Therefore, the proposed methods are convenient, rapid, sensitive, and reliable for the determination of trace SCs in wastewater.
研究领域:
环境分析化学
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药物代谢
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毒理学
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环境污染监测
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分子探针与检测技术
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产品关联
DOI
高影响因子
BMC Chemistry
·
2025
·Vol. 19
·期 1
·194
·
IF 4.6
Chenjian Zhou,Peiqi Wang,Jie Chen,Hualu Wu,Yige Yu
Parsaclisib is a novel, potent, highly selective, next-generation oral inhibitor of phosphatidylinositol 3-kinase δ (PI3Kδ) for patients with relapsed or refractory B-cell malignancies. However, there is no accurate and rapid method for the determination of parsaclisib. The aim of this study was to establish a rapid, specific and reliable ultra performance liquid chromatography tandem mass spectrometry (UPLC-MS/MS) method for the determination of parsaclisib, and to investigate in vitro metabolic stability using rat liver microsomes (RLMs) and in vivo pharmacokinetics in rats. Parsaclisib was detected by gradient elution on an Acquity UPLC BEH C18 column (2.1 mm × 50 mm, 1.7 μm) using acetonitrile and 0.1% formic acid as mobile phases, and pilaralisib was used as an internal standard (IS). Selective reaction monitoring (SRM) was used for detection. The method showed acceptable intra- and inter-day precision (< 8.6%) and accuracy (2.0–14.9%). The stability of the test samples was reliable during the analysis. In addition, the recoveries and matrix effects of the samples were within acceptable limits and were stable during storage and determination in rat plasma. The pharmacokinetic trend of parsaclisib in rats was also investigated by this newly developed assay after gavage administration of 2.0 mg/kg parsaclisib. Finally, i n vitro results showed that parsaclisib had a slow intrinsic clearance (Clint) value of 2.4 µL/min/mg protein with a half-life (t 1/2 ) value of 571.3 min. These findings theoretically supported the potential metabolism of parsaclisib in vivo.
研究领域:
药物分析
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药代动力学
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药物代谢
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分析化学
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肿瘤学
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生物分析方法开发
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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）