MICROCHEMICAL JOURNAL
·
2025
·
IF 5.1
Dong Wang,Mengrong Li,Tingting Dai,Xiangyu Zhang,Di Chen
A rapid, sensitive, and green sample preparation method based on polypropylene fiber-supported liquid-phase microextraction followed by liquid chromatography–tandem mass spectrometry was developed for the determination of tyrosine kinase inhibitors in plasma. Commercial oil absorbent pads composed of polypropylene fibers were used to support n-octanol as the extraction phase. The high chemical purity of the polypropylene fiber minimized background interference, enabling reliable trace-level analysis. The in-syringe format allowed simple push–pull operation, and extraction conditions were optimized for maximum efficiency. The method demonstrated excellent linearity (R 2 > 0.995), low limits of quantification (0.067–3.0 ng/mL), and high precision, with intra- and inter-day recoveries ranging from 79.5 % to 113.6 % and relative standard deviations below 14.2 %. A blinded spiked sample analysis confirmed the method’s reliability for clinical application. The greenness of the method, as evaluated by five green assessment tools, demonstrated excellent environmental compatibility. Overall, the proposed in-syringe polypropylene fiber-supported liquid-phase microextraction method offers a simple, cost-effective, and environmentally sustainable solution for the analysis of tyrosine kinase inhibitors in complex biological matrices.
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高影响因子
BMC Chemistry
·
2025
·Vol. 19
·期 1
·180
·
IF 4.6
Xiaoyu Yang,Wanling Lin,Yushang Zhao,Chaoyue Zhao,Fei Zhou,Dong Wang,Zhihong Yue,Lin Pei,Mei Jia,Bin Cao,Lin-Lin Cao,Hui Wang
“Xiannuoxin” (simnotrelvir/ritonavir) is a novel anti-severe acute respiratory syndrome coronavirus 2 (SARS-CoV-2) drug developed in China, which plays an antiviral role by inhibiting 3C-like protease (3CL pro ). At present, it has been put into clinical use, while a simple, accurate and sensitive detection method is urgently needed for the quantification of simnotrelvir/ritonavir in human serum and bronchoalveolar lavage fluid (BALF) to ensure safe and efficacious antiviral therapeutics. In this study, we developed a liquid chromatography tandem mass spectrophotometry (LC-MS/MS) method for the simultaneous determination of simnotrelvir, ritonavir and urea concentrations in human serum and BALF samples. Prior to LC-MS/MS analysis, a user-friendly, one-step pre-analytical process was conducted, followed by a rapid chromatographic run lasting 3 min. This was then succeeded by positive and negative electrospray ionization and detection using a triple quadrupole tandem mass spectrometer in the multiple reaction monitoring mode. Subsequently, the LC-MS/MS method underwent a comprehensive validation in aspects such as sensitivity (LoQs of 2.5 ng/mL, 0.1 ng/mL, and 1 μg/mL for simnotrelvir, ritonavir and urea), linearity, carryover, precision, trueness (recovery rates of simnotrelvir, ritonavir and urea were between 85 and 115%), matrix effect (within 85-115%) and stability (stable for 72 h at room temperature). The validation results demonstrated that this LC-MS/MS method was robust and reliable. Notably, we can use the urea dilution correction method to calculate the concentrations of simnotrelvir and ritonavir in epithelial lining fluid (ELF), which is of great significance for evaluating the effectiveness and safety of antiviral drug treatment.
研究领域:
药理学
·
分析化学
·
病毒学
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PubMed
高影响因子
Analytical Methods
·
2026
·
IF 2.6
Dandan Pan,Libang Chen,Haonan Luo,Haiyan Liu,Weihao Chen,Zhenzhou Jiang,Zhen Qiu,Nan Zhou,Yequan Zhou,Qiujin Xu,Tao Wang,Qian Lu,Tingting Yang
Our research team developed AB-38b, a biphenyl diester derivative containing α,β-unsaturated carbonyl groups, inspired by investigations into the pharmacological prevention and pathophysiology of diabetic kidney disease (DKD). We have completed the synthesis and pharmacodynamic evaluation of AB-38b in preclinical DKD studies. For pharmacokinetic analysis, we established a high-performance liquid chromatography-tandem mass spectrometry (HPLC-MS/MS) method for quantifying AB-38b in rat plasma, as well as in liver and kidney tissues. Sample preparation involved protein precipitation using methanol, with tolvaptan employed as the internal standard (IS). Chromatographic separation was achieved on a Shim-pack VP-ODS C18 column (2.0 × 150 mm, 5 µm), with mobile phase A (5 mM ammonium acetate) and mobile phase B (methanol) under gradient elution at a flow rate of 0.2 mL min−1. AB-38b and the IS were detected and quantified using positive electrospray ionization in multiple reaction monitoring (MRM) mode at transitions of m/z 705.30 → 618.20 for AB-38b and m/z 449.30 → 252.20 for the IS. The method demonstrated excellent linearity, stability, accuracy, precision, recovery, and a non-significant matrix effect within the validated range. A one-compartment model with rapid absorption and distribution, quicker elimination, and clear tissue distribution was demonstrated by the mean blood concentration–time curve of AB-38b in rat plasma. The liver tissue contained high levels of AB-38b, with no evidence of tissue accumulation observed. These findings offer a reference for further research into the pharmacological mechanisms and potential therapeutic applications of AB-38b in metabolically related diseases, especially DKD.
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高影响因子
MOLECULES
·
2018
·Vol. 23
·期 10
·2496
·
IF 3.098
Ying Zhou,Jian Guan,Weiwei Gao,Shencong Lv,Miaohua Ge
In this research, fifteen carbamate pesticide residues were systematically analyzed by ultra-high performance liquid chromatography–quadrupole-linear ion trap mass spectrometry on a QTRAP 5500 system in both multiple reaction monitoring (MRM) and enhanced product ion (EPI) scan modes. The carbamate pesticide residues were extracted from a variety of samples by QuEChERS method and separated by a popular reverse phase column (Waters BEH C18). Except for the current conformation criteria including selected ion pairs, retention time and relative intensities from MRM scan mode, the presence of carbamate pesticide residues in diverse samples, especially some doubtful cases, could also be confirmed by the matching of carbamate pesticide spectra via EPI scan mode. Moreover, the fragmentation routes of fifteen carbamates were firstly explained based on the mass spectra obtained by a QTRAP system; the characteristic fragment ion from a neutral loss of CH3NCO (−57 Da) could be observed. The limits of detection and quantification for fifteen carbamates were 0.2–2.0 μg kg−1and 0.5–5.0 μg kg−1, respectively. For the intra- (n =3) and inter-day (n =15) precisions, the recoveries of fifteen carbamates from spiked samples ranged from 88.1% to 118.4%, and the coefficients of variation (CVs) were all below 10%. The method was applied to pesticide residues detection in fruit, vegetable and green tea samples taken from local markets, in which carbamates were extensively detected but all below the standard of maximum residue limit.
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Talanta Open
·
2026
·
IF 5.1
Jie Fu,Yong Shao,Hua Shao,Guo Jingyuan,Tangwei Zhang,Jin Fen,Jing Wang,A.M. Abd El-Aty,Yongxin She
A rapid, sensitive, and reliable method was developed for the determination of six dinocap phenol isomers in 23 plant-derived foods via a modified QuEChERS approach coupled with liquid chromatography‒tandem mass spectrometry (LC‒MS‒MS/MS). Chromatographic and mass spectrometric conditions were optimized, and the separation performance of eight chromatographic columns was systematically evaluated to achieve effective isolation of the six dinocap phenol isomers. The method was validated on the basis of maximum residue limits (MRLs) across 23 matrices, with spiked levels ranging from 0.003 to 0.3 mg/kg. The average recoveries were between 60% and 112%, with relative standard deviations (RSD) less than 21%. The limits of quantification (LOQs) ranged from 0.003 to 0.015 mg/kg. This method successfully addressed challenges in the detection of dinocap phenols by enabling clear and precise separation of individual isomers while mitigating matrix effects through matrix-matched calibration.This study contributes to global efforts to increase food safety, support sustainable agricultural practices, and promote public health through improved methods for detecting and managing pesticide residues.
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高影响因子
EUROPEAN JOURNAL OF MASS SPECTROMETRY
·
2019
·
IF 0.851
Shencong Lv,Henghui Wang,Yong Yan,Miaohua Ge,Jian Guan
A simple, rapid, and efficient liquid chromatography tandem mass spectrometry (LC–MS/MS) method, operated in electrospray ionization and quadrupole linear ion trap modes, has been developed for the identification and structural characterization of aflatoxins in peanuts and its derivative products or bean sauce. Samples (5 g) were extracted with acetonitrile/water/formic acid (79:20:1, v/v). After centrifugation and dilution, the extracts were separated on a C18 analytical column by gradient elution (acetonitrile/0.2% formic acid) and analyzed by UPLC–MS/MS. External calibration was used for qualification. The developed multiple reaction monitoring–information-dependent acquisition–enhanced product ion method enabled quantification and confirmation of the analytes in a single run. Enhanced product ion mode was used for qualitative analysis, while multiple reaction monitoring mode was used for quantitative analysis. An in-house library was constructed for identification. Calibration curves showed good linearity with correlation coefficients (r) higher than 0.994. Limits of detection were determined to be below 0.26 µg kg−1 for most analytes. The recoveries for those substances were in the acceptable range of 80.2%–119.1%. A new LC–MS3 method was established for further confirmation. One pickled pepper peanut was found to contain aflatoxins B1, B2, and G1 with contents of 90.93, 26.64, and 1.92 µg kg−1, respectively.
研究领域:
食品安全
·
分析化学
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JOURNAL OF CHROMATOGRAPHY B-ANALYTICAL TECHNOLOGIES IN THE BIOMEDICAL AND LIFE SCIENCES
·
2019
·
IF 2.813
Tengfei Li,Bin Huang,Duo Li,Yantong Zhu,Li Ding,Chang Shu
In this work, we developed and validated the specific, sensitive and simple LC–MS/MS method for quantification of eslicarbazepine in human plasma. The analyte samples were prepared through a simple one-step protein precipitation method by acetonitrile . The chromatographic separation was operated on an economical Hanbon ODS-2 C18 column (150 mm × 2.1 mm, 10 μm) with isocratic elution using 10 mM ammonium acetate containing 0.01% formic acid and acetonitrile (72:28, v/v) as the mobile phase at the flow rate of 0.5 mL/min. The mass quantification was carried on the multiple reaction monitoring (MRM) of the transitions of m / z 255.1 → 194.1 for eslicarbazepine and m / z 446.1 → 321.1 for glipizide (the internal standard), respectively. The established method was validated with acceptable specificity, linearity, accuracy, precision, extraction recovery, matrix effect and stability in accordance with FDA regulations. At last, the validated method was successfully applied to determination of eslicarbazepine in human plasma obtained from clinical study.
研究领域:
药物分析
·
临床药理学
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PubMed
高影响因子
FOOD AND AGRICULTURAL IMMUNOLOGY
·
2021
·
IF 3.101
Enhui Guo,Linchuan Zhao,Kang Wu,Wen Huang,Kang Zhao,Jianguo Li,Anping Deng
Amphenicol antibiotics including chloramphenicol (CAP), florfenicol (FF) and thiamphenicol (TAP) have been widely used in aquaculture and veterinary to treat various infections. Because of their high toxicity, it is important to detect these amphenicol antibiotics simultaneously. Using the monoclonal antibody against CAP (mAbCAP) binding CAP only and the mAbFF recognizing both FF and TAP, the two antibodies were covalently coupled to CNBr-activated Sepharose-4B for the simultaneous extraction of CAP, FF and TAP from samples. The bound CAP, FF and TAP were eluted from the Sepharose-4B and measured by LC–MS/MS. The extraction conditions of the two-antibodies-immobilized immunoaffinity clean-up (IAC) for CAP, FF and TAP were optimized and the maximum capacity was investigated. The extraction efficiency of IAC for CAP, FF and TAP was 1.1–2.1 times higher than that of SPE. The LC–MS/MS coupled with IAC was a powerful analytical method for the detection of CAP, FF and TAP simultaneously.
研究领域:
分析化学
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环境科学
·
兽医学
·
食品安全
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高影响因子
JOURNAL OF PHARMACEUTICAL AND BIOMEDICAL ANALYSIS
·
2016
·
IF 3.169
Yidi Yang,Xi Zhu,Fei Zhang,Wei Li,Ying Wu,Li Ding
Stress testing was carried out under acidic, alkaline, oxidative, thermal and photolytic conditions to evaluate the intrinsic stability of posaconazole injection. A total of four degradation products were detected and the drug was found to be susceptible to oxidative and thermal degradations. Three unknown degradants formed under oxidative stress condition were isolated by preparative HPLC and unambiguously elucidated by LC–TOF/MS, LC–MS/MS, 1 H NMR, 13 C NMR and 2D NMR techniques. Based on the spectrometric and spectroscopic information, these novel degradation products were unequivocally assigned as the N-oxides of posaconazole. Probable mechanisms for the formation of the degradants were proposed. A new and selective HPLC method was developed and validated to separate, detect and quantify all the degradants in posaconazole injection.
研究领域:
药物分析
·
药学
·
质谱分析
·
核磁共振
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PubMed
高影响因子
JOURNAL OF CHROMATOGRAPHY B-ANALYTICAL TECHNOLOGIES IN THE BIOMEDICAL AND LIFE SCIENCES
·
2023
·
IF 3
Zheyue Bo,Wanjun Han,Haoyue Zhao,Han Liu,Ting Liang,Lanjing Li,Taotao Peng,Ying Li,Chunshan Gui
Cypate, a heptamethine cyanine dye, is a prototypic near-infrared (NIR) theranostic agent for optical imaging and photothermal therapy. In the present study, a selective, sensitive, and rapid liquid chromatography-tandem mass spectrometry (LC-MS/MS) method was developed and validated for the quantitation of cypate in mouse plasma. The chromatographic separation was achieved using a short C 18 column (2.1 mm × 50 mm, 5 μm) with a run time of 5 min. The MS was operated in multiple reaction monitoring (MRM) mode via positive electrospray ionization. The ion transitions for cypate and internal standard IR-820 were m / z 626.3 → 596.3 and m / z 827.4 → 330.2, respectively. The method was linear over a concentration range of 1.0–500 ng/mL. The within-run and between-run precision was less than 14.4% with accuracy in the range of −13.4% ∼ 9.8%. The validated method was successfully applied to a pharmacokinetic study of cypate in mice following intravenous administration.
研究领域:
分析化学
·
药理学
·
医学
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PubMed
高影响因子
JOURNAL OF PHARMACEUTICAL AND BIOMEDICAL ANALYSIS
·
2025
·
IF 3.1
Jiangbin Han,Lijuan Zhai,Jie Wang,Biying Dai,Huiyue Lu,Jiao Chen,Xiaoli Wang,Yuyu Wu,Wen Qian
Hetrombopag (Hengqu®) is an oral nonpeptide thrombopoietin receptor agonist for the treatment of thrombocytopenia and aplastic anemia. Research on the pharmacokinetic behavior is very important, but accurate quantification of metal-sensitive hetrombopag in biological specimens is a challenging analytical problem. In view of the presence of trace metals from a variety of sources, such as chromatographic system, containers, and the mass spectrometry spray needle, which can contribute to poor peak shape, tailing, and diminished recovery of compound. To ameliorate these problems, different solvent additives, mobile phase, containers and precipitant reagents were investigated to reduce the negative effects. In the present study, a robust, selective, and sensitive liquid chromatography–tandem mass spectrometry (LC-MS/MS) method for the determination of hetrombopag in dog plasma was developed based on the dual strategies: (1) 6 % perchloric acid in acetonitrile eliminates metal ion adsorption in storage containers, and (2) 0.01 % trifluoroacetic acid (TFA) in the mobile phase suppresses chelation in chromatographic systems. These two solvents are essential requirements for ensuring stable analytical signals. This method employed an InfinityLab Poroshell 120 EC-C18 column (4.6 ×50 mm, 2.7 μm, Agilent) with a gradient system comprising 0.01 % trifluoroacetic acid with 10 mM ammonium formate (phase A) and a mixture of H 2 O: methanol: isopropanol (1:10:10, v/v/v) containing 0.01 % trifluoroacetic acid and 10 mM ammonium formate (phase B). The column temperature of 50℃ and the addition of isopropanol were beneficial for the separation of interfering peaks and target analyte peaks in plasma. The method exhibits excellent linearity over 3 orders of magnitude. The method achieved a lower limit of quantification (LLOQ) of 0.10 ng/mL using only 50 μL of plasma, with precision (RSD ≤ 8.83 %) and accuracy (88.4–102.2 %) within acceptable limits. The method was applied to determine the plasma concentration of hetrombopag in eight male beagle dogs after each administration of three 2.5 mg hetrombopag tablets. The analytical methodology described in the present work should be useful in the future work aiming to establish a model relating metal-sensitive other compounds.
研究领域:
分析化学
·
药代动力学
·
生物分析
·
质谱分析
·
药物研发
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高影响因子
ANALYTICAL AND BIOANALYTICAL CHEMISTRY
·
2024
·Vol. 416
·期 29
·7043-7062
·
IF 3.8
Liu Wen-Ya,Xu Di,Meng Hui-Hui,Wang Cheng-Yao,Feng Xin,Wang Jun-Song
Cucurbitacin B (CuB) is a natural triterpenoid with diverse pharmacological effects including potent anticancer activity. However, its oral bioavailability is hampered by limited metabolism in vivo. We characterized CuB’s in vivo metabolism in rats to uncover bioactive metabolites retaining therapeutic potential, using a robust UHPLC-Q-TOF–MS/MS workflow. This workflow combined molecular networking, fragmentation filtering, and mass defect filtering to identify CuB metabolites in rat urine, plasma, and feces following oral administration. Thirteen metabolites were identified and seven were confirmed. Major phase I transformations involved hydrolysis, reduction, epoxidation, and amination. Phase II conjugation included cysteine, glutathione, glucuronide, and gluconic acid conjugates. Notably, one of the main metabolites formed was the cysteine conjugate CuB-Cys. CuB-Cys maintained similar in vitro antiproliferative activity to CuB on HepG2, MCF-7, and PANC-1 cancer cell lines. However, it demonstrated lower cytotoxicity towards non-cancerous L02 cells, highlighting improved therapeutic selectivity. Mechanistically, CuB-Cys induced greater apoptotic signaling in HepG2 cells than CuB via enhanced caspase activation and disrupted BAX-Bcl-2 balance. This represents the first systematic characterization of CuB’s in vivo metabolic pathway. The identification and confirmation of CuB-Cys provide insight for drug development efforts aiming to maintain therapeutic efficacy while reducing toxicity, via metabolite-based approaches. Our findings shed light on strategies for improving CuB’s clinical potential. Graphical Abstract
研究领域:
药理学
·
代谢组学
·
肿瘤学
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PubMed
高影响因子
危险品化学品经营许可证（带存储）