Results in Chemistry
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2025
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IF 4.2
Oushan Tang,Shitong Wang,Guanguan Qiu,Majun Zhang,Liping Ling,Yan Zhang,Meiqun Guo,Chunxia Shen,Bin Quan,Hongjie Lang,Qing Shen,Keyun Cheng
This study proposes a method combining the Captiva enhanced matrix removal (EMR)-Lipid solid-phase extraction column with ultra-performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS) for the qualitative and quantitative analysis of five common oral anticoagulants (OACs) (rivaroxaban, apixaban, edoxaban, dabigatran, and warfarin) in plasma samples. The method, through a simplified sample pretreatment, significantly enhances the recovery rate of OACs (ranging from 88% to 96%), demonstrating superior purification effects compared to traditional solid-phase extraction methods, and effectively removes matrix interference. The method exhibits good linearity over a concentration range of 0.010 to 5.0 × 10 2 ng·mL −1 (r 2 = 0.9514 to 0.9998), with high sensitivity, detection limits of 0.010 to 0.10 ng·mL −1 , and quantification limits of 0.10 to 1.0 ng·mL −1 . The recovery and precision analysis indicate that the method is highly accurate and stable, suitable for the analysis of large batches of plasma samples containing OACs. This method provides an efficient and reliable testing tool for clinical drug monitoring, contributing to the optimization and enhancement of safety in personalized anticoagulation therapy.
研究领域:
临床药理学
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药物代谢
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分析化学
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个体化医学
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毒理学
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生物分析
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抗凝治疗
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JOURNAL OF CHROMATOGRAPHIC SCIENCE
·
2021
·Vol. 60
·期 2
·186-193
·
IF 1.618
Liu Ruichen,Liang Huiliang,Li Zhen,Zang Hengchang
Qilong capsule (QLC) is a well-known Traditional Chinese Medicine, and it has a long history for the treatment of ischemic stroke. Its major ingredients are saponins, such as paeoniflorin, amygdalin and calycosin-7-glucoside, contributing to vasodilation function. In this study, a simple, rapid and sensitive high-performance liquid chromatography-tandem mass spectrometry method was developed to determine three bioactive ingredients in rat plasma after oral administration of QLC. A simple acetonitrile precipitation method was introduced during the sample preparation. Chromatographic separation was performed on a Shiseido CAPCELL PAC MGIII-C18 column using a gradient elution with acetonitrile and water (0.1% formic acid) as a mobile phase, and the chromatographic separation was 5 min. The methodological evaluation showed that this method had a high sensitivity (the lower limit of quantification was 1 ng/mL for calycosin-7-glucoside, 5 ng/mL for paeoniflorin, 5 ng/mL for amygdalin), satisfactory accuracy (relative error ≤ ±15%) and precision (relative standard deviation ≤15%). Then, the analytical method was applied to the pharmacokinetic study in rats following oral administration of the extracts in QLC. Meanwhile, the pharmacokinetic parameters of complex system in QLC were analyzed and the potential interaction between ingredients was explored. The present quantification method and pharmacokinetic study will provide a meaningful reference for the formulas research of QLC in the treatment of ischemic stroke.HighlightA simple, rapid and sensitive HPLC–MS/MS analytical method was developed for the simultaneous determination of three ingredients in rat plasma after oral administration of QLC.A simple acetonitrile precipitation method was introduced to extract three biomedical ingredients during the plasma sample preparation.The pharmacokinetic results revealed the pharmacological active substances, identified internal variation rules and provided a meaningful reference for the formulas research of QLC in the treatment of ischemic stroke.
研究领域:
中药学
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药理学
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分析化学
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PubMed
高影响因子
ACS Omega
·
2026
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IF 5.2
Benkai Qin,Huina Zhang,Hangyu Zhao,Yuchen Su,Yifu Kong,Shengshuo Zhang,Luwei Wang,Yonghua Yu,Jie Gu,Tingting Lou
Perospirone hydrochloride hydrate is an atypical antipsychotic widely used in the management of schizophrenia. Reliable quantification of its plasma concentrations remains essential for pharmacokinetic characterization and dose optimization. A rapid, specific, and sensitive liquid chromatography–tandem mass spectrometry (LC–MS/MS) method was developed and fully validated for the quantification of perospirone in human EDTA–K2 plasma using perospirone-d8 as the internal standard (IS). Chromatographic separation was achieved on a Kinetex C18 analytical column (100 Å, 50 mm × 2.1 mm, 5 μm, 100 Å). The mobile phase consisted of an aqueous solution of 0.1% formic acid and 1 mM ammonium formate (MPA) and a solution of 95% acetonitrile containing 0.1% formic acid and 1 mM ammonium formate (MPB), delivered at a flow rate of 0.300 mL/min. The injection volume was 10 μL. Mass spectrometric detection was performed using electrospray ionization in positive-ion mode with multiple reaction monitoring (MRM). The method exhibited linearity over a concentration range of 0.0200–12.0 ng/mL. The validated method was successfully applied to fasting and postprandial pharmacokinetic studies following oral administration of perospirone hydrochloride tablets. The method demonstrates strong performance characteristics and practical utility, supporting its application in pharmacokinetic investigations, bioequivalence assessment, and clinical drug monitoring.
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JOURNAL OF CHROMATOGRAPHY A
·
2026
·
IF 4
Mantang Chen,Libin Wan,Shuhan Yu,Li Chen,Jingjing Yu,Xiaoyu Wang,Cong Nie,Fuwei Xie,Wenfen Zhang
Simple and convenient synthesis of a purification material of CZIFA. • Enhanced purification performance of CZIFA by acid treatment strategy. • Analysis and detection of pesticide residues in complex matrices. • Expanded application of ZIF-derived carbon materials in food safety detection. Porous carbon-based QuEChERS purification material (CZIFA) was synthesized through a straightforward calcination and acid treatment process using Zeolitic Imidazolate Framework-67 (ZIF-67) as the precursor. The abundant adsorption sites and excellent clean-up capability of CZIFA resulting from acid treatment were confirmed through a series of characterization and performance evaluations. Combined with LC-MS/MS, a modified QuEChERS method using CZIFA as the adsorbent was developed for the simultaneous detection of 48 pesticide residues in tobacco. Under optimized conditions, the established method achieved low limits of detection (0.02–9.92 μg/kg), wide linear ranges (2–200 μg/L), and satisfactory precision. The average recoveries of the method were in the range of 80.1–119.7% with the relative standard deviations (RSDs) of <9.5%. This study provides a novel and efficient functionalized material for analyzing pesticide residues in complex matrices. Especially, it expands the application of ZIF-derived carbon materials in food safety detection. Download: Download high-res image (298KB) Download: Download full-size image
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Forensic Toxicology
·
2025
·
IF 3
Zhang Aijia,Ye Shuang,Liu Zilong,Tan Lingzhi,Liang Man
Purpose Regional traditional plant khat, which have been recreationally used world-wide recently, has been proven to be a mixture of several biologically active ingredients. Herein, a chosen specimen, vitreous humor (VH) and a novel pretreatment, electromembrane extraction (EME), are applied for forensic investigations of such abused plant. Methods VH, as an alternative matrix, is being used for evaluating possible compounds more and more; EME, a novel and efficient pretreatment method, is applied to detect the ingredients from natural complex matrices with advantages of a more sustainable microextraction technique. This study aims to analyze the ingredients of khat, norephedrine (NE), norpseudoephedrine (NPE) and cathinone (CTN), as well as their concentrations in VH of khat-treated mice applying EME. Results After optimization, 2-ethylnitrobenzene (ENB)/undecanol was used as the support liquid membrane (SLM), HCl (pH = 2) as the acceptor solution, extraction voltage at 60 V, and extraction time for 30 min. The established EME was combined with liquid chromatography–ultraviolet spectrometry (LC–UV) and liquid chromatography–tandem mass spectrometry (LC–MS/MS) to evaluate spiked VH. The LOD of NE, NPE, and CTN were 0.40–1.90 µg/mL with linearity ( R 2 > 0.9624) and repeatability (< 13%). Conclusions By this method, NE, NPE, and CTN were detected to be 14.4 ± 0.54 µg/mL, 8.50 ± 0.69 µg/mL, and 90.5 ± 7.88 µg/mL in VH of mice administrated with khat for 28 days.
研究领域:
法医学
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分析化学
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药理学
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PubMed
高影响因子
MICROCHEMICAL JOURNAL
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2025
·
IF 5.1
Liang Li,Meijia Liu,Wei Long,Wanting Gao,Xinyan Chen
Phthalates (PAEs), including dimethyl phthalate (DMP), diethyl phthalate (DEP), benzyl butyl phthalate (BBP), dibutyl phthalate (DBP), di-n-octyl phthalate (DNOP), and di(2-ethylhexyl) phthalate (DEHP), are well-documented endocrine-disrupting chemicals posing significant environmental and health risks. To address the limitations of conventional detection methods, we developed a novel core-shell magnetic covalent organic framework (Fe₃O₄@TAPOB-COF) via a multi-step synthesis protocol involving solvothermal reactions, silica coating, amino functionalization, and Schiff-base condensation. Comprehensive characterization using FTIR, XRD, SEM/TEM, and VSM confirmed the successful formation of a 25 nm crystalline COF shell with preserved superparamagnetism (12.7 emu/g), exceptional thermal stability (<10 % capacity loss at 300 °C), and broad pH tolerance (pH 2.0–11). When employed for magnetic solid-phase extraction (MSPE) of the six target PAEs, the material exhibited outstanding performance with detection limits of 0.14–22 ng/L and quantification limits of 0.46–73 ng/L, demonstrating wide linear ranges (1.0–1000 μg/L, R > 0.999) and excellent precision (intra-day RSD 4.9–9.1 %; inter-day RSD 7.3–13.5 %). The extraction mechanism, driven by synergistic π–π interactions and hydrophobic effects, achieved adsorption capacities of 312–1110 μg/g. In real water samples, consistent recoveries of 66.5–113.1 % were obtained with >75.0 % efficiency retention after six regeneration cycles, while complete extraction of BBP/DBP and 91.8 % removal of high-concentration DNOP (4600 μg/L) were achieved in industrial wastewater applications. Compared to conventional methods (SPE-GC–MS, LLE-LC–MS), this approach reduced solvent consumption by 80.0 %, improved throughput fivefold, and achieved detection limits 2–4 orders of magnitude lower than EPA Method 8061. The developed method establishes a robust, sensitive, and environmentally friendly analytical platform for trace-level PAE monitoring, offering significant advancements in environmental pollution control through enhanced sensitivity, cost-effectiveness, and operational efficiency.
研究领域:
环境化学
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分析化学
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材料科学
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毒理学
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水污染控制
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高影响因子
JOURNAL OF SEPARATION SCIENCE
·
2025
·Vol. 48
·期 2
·e70100
·
IF 2.8
Liang Li,Rendan Zhou,Huiying Xie,Gang Li,Zhiguang Xu,Meijia Liu,Wanting Gao
The widespread use of organophosphorus pesticides (OPs) has raised significant environmental and health concerns due to their residues in soil and potential entry into the food chain. This study introduced chiral analysis methods for four OPs—methamidophos (METHP), dipterex (DIP), malathion (MALA), and isothiophos-methyl (ISOME)—using liquid chromatography–tandem mass spectrometry (LC–MS/MS) with cellulose-based chiral columns. Three distinct methods were established: one for METHP, another for DIP, and a third for MALA and ISOME. Key chromatographic variables, including organic mobile phases and column temperatures, were systematically optimized, achieving maximum resolutions ( R s) of 1.61 for METHP, 2.40 for DIP, 1.70 for MALA, and 2.02 for ISOME. The QuEChERS method was employed for sample pretreatment, ensuring high recoveries. All three methods demonstrated excellent linearity ( R > 0.998), accuracy with recoveries ranging from 79% to 121%, precision with RSD% < 11%, and sensitivity with low limits of enantiomer detection (LODs) as low as 0.17 µg/kg for METHP, 0.087 µg/kg for DIP, 0.062 µg/kg for MALA, and 0.054 µg/kg for ISOME, representing a sensitivity improvement of 16–172 times compared to existing methods. Field soil samples from Yangzizhou District, Nanchang, China, revealed significant contamination by ISOME, with concentrations of a single enantiomer reaching up to 8343 µg/kg, while MALA exhibited varying enantiomeric ratios with depth. This study provides robust analytical tools for monitoring chiral OP residues in soil, contributing to food safety and environmental protection.
研究领域:
环境科学
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分析化学
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食品安全
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PubMed
高影响因子
Animals
·
2025
·Vol. 15
·期 7
·950
·
IF 2.7
Feifei Zhao,Changcheng Lin,Yunying Wu,Xinyue Luo,Ning Han,Wenguang Xiong,Zhenling Zeng
Simple SummaryGabapentin is an analogue of the neurotransmitter γ-aminobutyric acid, which is commonly used to treat neuropathic pain and epilepsy. However, studies have shown that early use of gabapentin can significantly reduce cats’ stress and increase their compliance with veterinary examinations. There is currently little research on the pharmacokinetics of gabapentin tablets for oral administration in cats. Consequently, monitoring gabapentin plasma levels provides critical insights into therapeutic adherence and facilitates early identification of toxicity thresholds. In this study, a novel LC-MS/MS assay was established and comprehensively validated to achieve high-throughput quantification of gabapentin in feline plasma resolution within 7 min. Additionally, this study provides further clinical evaluation for the management of sedation and anti-stress in cats.Gabapentin (GBP), a γ-aminobutyric acid analogue used for neuropathic pain and epilepsy, can reduce cat stress and improve veterinary exam compliance. A sensitive LC-MS/MS assay was established and rigorously validated for quantifying GBP in feline plasma. The method employed acetonitrile-mediated protein precipitation to efficiently extract GBP and its internal standard, pregabalin (PGB). Chromatographic separation was achieved within 7 min using a C18 column (2.1 × 50 mm, 1.7 μm) with a gradient mobile phase comprising 0.1% (v/v) formic acid in water and acetonitrile. The pharmacokinetics of 25 mg/kg GBP was studied by single-dose oral and intravenous administration. The results demonstrated that the method exhibited satisfactory precision, accuracy and linearity. The pharmacokinetic results showed that the Tmax, Cmax, T1/2and AUC0–tof GBP in cats after oral administration of 25 mg/kg were (1.83 ± 0.75) h, (13.94 ± 3.75) μg/mL, (5.60 ± 1.79) h and (115.54 ± 27.56) (μg/mL) h, respectively. The results of the study indicated that after intravenous administration of 25 mg/kg GBP, the C0, T1/2and AUC0–twere (58.82 ± 15.34) μg/mL, (3.87 ± 0.64) h and (160.44 ± 32.65) (μg/mL) h, respectively. The oral bioavailability of GBP in cats was (78.71 ± 18.55)%. In this study, a selective and sensitive LC-MS/MS method for the quantification of GBP in cat plasma was developed and validated. This method was successfully employed to assess the pharmacokinetics following the oral and intravenous administration of GBP in cats.
研究领域:
兽医学
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分析化学
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药理学
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PubMed
高影响因子
Food Analytical Methods
·
2024
·
IF 2.6
Pan Xingyu,Chen Jinzi,Guo Tao,Kuang Fengjiao,Kang Zonghua,Luo Jianguang
Betel nut (Areca nut, AN) products are extensively consumed across East and South Asian countries, with Binglang being the predominant chewable AN product in China. Given the increased risk of carcinogenicity associated with alkaloid nitrogen oxides compared to the primary alkaloids in AN, this study aimed to establish a precise and sensitive method for quantitative analysis of the arecoline N-oxide (ACNO) and arecaidine N-oxide (ADNO) at three different processing stages of Binglang using liquid chromatography-tandem mass spectrometry (LC–MS/MS). The developed method underwent comprehensive validation, evaluating key analytical parameters including selectivity, linearity, sensitivity, accuracy, precision, and stability. Notably, the method demonstrated excellent sensitivity, with the limits of detection (LOD) ranging from 0.029 to 0.135 ng/mL, while the limits of quantification (LOQ) ranging from 0.095 to 0.450 ng/mL. Subsequently, the established analytical technique was applied to analyze 15 Binglang samples at three different processing stages, providing the first evidence of the content and variability of alkaloid nitrogen oxides throughout these stages. ACNO and ADNO were detected in all samples, and their total contents ranged from 4.31 to 32.82 μg/g. The changes observed across different processing stages indicated that the roasting process at 80 ℃ resulted in the promotion of alkaloid nitrogen oxides. This analytical approach constitutes a valuable tool for the quality control and risk assessment of Binglang and can be extended to other AN products, thereby assisting in addressing health concerns associated with these products.
研究领域:
药理学
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分析化学
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食品安全
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高影响因子
JOURNAL OF PHARMACEUTICAL AND BIOMEDICAL ANALYSIS
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2022
·
IF 3.571
Xiaoli Zhang,Na Yang,Min Wang,JiaJia Ge,Huaijun Zhu,Jun He,Weihong Ge
Gestational diabetes mellitus (GDM) is not only a threat to the health of pregnant women, but also has profound effects on the health of offspring. Studies have shown that the imbalance of estrogen metabolism is associated with an increased risk of GDM. In this study, an ultra-performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS) method was established and validated for simultaneous quantification of thirteen estrogens in the urine of GDM women, including estrone (E1), estradiol (E2), estriol (E3), and their hydroxylated and methylated metabolites. The method was achieved on a Waters CORTECS C18 column (2.1 mm × 150 mm, 1.6 µm) within 8.5 min. The linear range of thirteen estrogens in urine was 2–1000 pg·mL −1 . Both intra- and inter-day precision for each analyte were less than 15%, with accuracies ranging from 8.3% to 7.3%. The extraction recoveries rate were between 86% and 111%, and stability verification results met the requirements for determination of biological samples. The results suggested that the concentrations of estrogens in all urine samples range from 0.08 to 134.06 (pg·mg −1 creatinine). The mean levels of E1, E2 and most estrogen metabolites in the urine of GDM women were higher than those in healthy pregnant women. Notably, the mean level of 2-hydroxyestrone (2-OHE1) in GDM women was 13.2-fold lower than that in healthy pregnant women. The types of estrogens with the highest mean levels in the urine of GDM and healthy pregnant women were obviously different, which are 2-methoxyestrone (2MeOE1) and E3, respectively. Our results demonstrated that this specific and sensitive method is suitable for quantifying estrogens in human urine and could provide support for further research on estrogen-related pathological mechanisms in GDM and other diseases.
研究领域:
医学
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内分泌学
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分析化学
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DOI
PubMed
高影响因子
JOURNAL OF MASS SPECTROMETRY
·
2026
·Vol. 61
·期 5
·e70057
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IF 2.1
Daomiao Huang,Hong Chen,Hai Zhang,Xin Dong
In assisted reproductive technology (ART), controlled ovarian hyperstimulation (COS) plays an important role in guiding treatment progress and determining success. Many ovulation-inducing agents are used in this process, including human menopausal gonadotropin (HMG), recombinant follicle-stimulating hormone (r-FSH), recombinant luteinizing hormone (r-hLH), urinary human chorionic gonadotropin (u-hCG), and recombinant human chorionic gonadotropin (r-hCG). HMG, which comes from the urine of postmenopausal women, mainly contains FSH, LH, and hCG. While bioactivity-based potency units and immunoassay-based ELISA methods remain the gold standard for quantifying protein therapeutics, LC–MS/MS is emerging as a game-changing technology. Its unique strengths are exceptional specificity and absolute quantification capabilities, independence from specialized reagents, powerful multiplexing potential, and ability to provide structural insights, establishing it as an essential tool for both orthogonal verification and cutting-edge research in the field. This study used reverse-phase liquid chromatography with mass spectrometry (RP-LC–MS/MS) and a label-free quantitative proteomics method to analyze imported r-hFSH, r-hLH, r-hCG (Gonal-F, Luveris, and Ovidrel), three domestic HMG products (Le Baode, Man Fuxin, and Xin Yunle), and u-hCG (Li Zhu). The results showed that the purity of the main component in imported gonadotropin drugs was higher than 98.55%. On the other hand, the main element of domestic u-HMG is FSH, with small amounts of hCG and very little LH. These results reveal significant differences in the composition of imported and domestic gonadotropin products, underscoring the need to further evaluate their biological activity and clinical effectiveness. This study provides important insights into drug selection for ART, with practical value for improving the quality of HMG drugs and making better use of them in clinical settings.
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JOURNAL OF PHARMACOLOGICAL AND TOXICOLOGICAL METHODS
·
2026
·
IF 2.1
Zhenhua Zhang,Bingchen Ge,Yanyu Wang,Changrui Long,Huixing Wu,Hui Chen,Shijian Xiang,Benjie Zhou
Objective To develop a novel approach for quantitative analysis of three pharmaceutical agents commonly employed in the treatment of hematological disorders (venetoclax, busulfan, and voriconazole) by liquid chromatography tandem mass spectrometry (LC-MS/MS). Methods The internal standards were venetoclax-d8 (venetoclax), busulfan-d8 (busulfan), and posaconazole (voriconazole), which were separated on a Phenomenex Kinetex® C 18 (2.1 × 50 mm, 2.6 μm) column, and the multiple reaction monitoring was carried out in the positive ion mode of the SCIEX Triple Quad™ 5500. Protein precipitation pretreatment was performed using acetonitrile, with solvent A (2 mmol/L ammonium acetate dissolved in water containing 0.1% formic acid) and solvent B (acetonitrile solution containing 0.1% formic acid) as mobile phases. The flow rate was 0.8 mL/min, and the injection volume was 5 μL. Results The method was validated with regards to selectivity, lower limit of quantification, linearity, precision and accuracy, matrix effect and extraction recovery, dilution integrity, and stability. The runtime of each plasma sample was 3.1 min. The concentration ranges of the calibration curves were 50–10,000 ng/mL for venetoclax and voriconazole, and 15–3000 ng/mL for busulfan, with all the three correlation coefficients greater than 0.999. There were significant drug–drug interactions with venetocalx and voriconazole, and the incidence of adverse reactions was related to the venetoclax exposure in vivo. Concentrations of busulfan and voriconazole showed substantial interindividual variability. Conclusion This study develops, with validation, a novel LC-MS/MS method for simultaneous determination of venetoclax, busulfan, and voriconazole, which is suitable for application to therapeutic drug monitoring in patients with acute myeloid leukemia.
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