JOURNAL OF PHARMACOLOGICAL AND TOXICOLOGICAL METHODS
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2026
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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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Biosensors-Basel
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2026
·Vol. 16
·期 6
·311
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IF 6.2
Xiqiong Mu,Yaqin Dong,Ling Jin,Tiantian Zhu
This study compares the performance of novel fluorescent nanobiosensors and liquid chromatography–mass spectrometry (LC-MS) for detecting organophosphorus pesticide residues inAngelica sinensis. Key parameters such as recovery rate and relative standard deviation (RSD) were evaluated to identify a preferable detection method. The results show that the fluorescent nanobiosensor offers superior sensitivity, whereas LC-MS excels in accuracy and quantitative analysis. For phoxim, the GQDs@GSH sensor achieved an LOD of 0.075 μmol·L−1, with recoveries of 97.65–100.62% (RSD < 3.35%). For glyphosate, the PDOA/Cu2+sensor achieved an LOD of 1.8 nmol·L−1, and the AgNCs sensor achieved an LOD of 21 nmol·L−1, with recoveries of 91.30–105.34% (RSD < 3.35%). The originality of this work is threefold and does not claim de novo synthesis of unknown materials: (i) it is the first validation of three existing fluorescent nanosensors (GQDs@GSH, PDOA/Cu2+, and AgNCs) specifically for organophosphorus pesticide detection in the complex medicinal plant matrixAngelica sinensis; (ii) it provides the first systematic comparison of these nanosensors against the pharmacopeia-standard LC-MS method in this matrix, delineating their complementary advantages; (iii) it is the first assessment of their phytotoxicity inAngelica sinensisseedlings, demonstrating biocompatibility and potential for in planta imaging.
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Forensic Toxicology
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2025
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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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MICROCHEMICAL JOURNAL
·
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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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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Frontiers in Veterinary Science
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2025
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IF 2.9
Shujun Shi,Yulan Feng,Lina Zhu,Zhenghan Chen,Qiao Li,Rui Zhang,Xuejiao An,Yaojing Yue
The epididymis is a crucial organ for sperm maturation and storage, with metabolic microenvironmental differences across its functional segments (Caput, Corpus, Cauda) being pivotal to this process. However, the underlying metabolic regulatory mechanisms remain incompletely defined. This study systematically characterized region-specific metabolic profiles in the epididymis of Hu sheep and elucidated their functional associations with sperm maturation. Tissues from the caput, corpus, and cauda of the epididymis from eight Hu rams were subjected to untargeted metabolomic analysis using UHPLC-Q-Exactive HF-X. Differential metabolites were screened by combining multivariate statistical analysis (OPLS-DA, VIP >1) and univariate statistical analysis (student t -test, p < 0.05), with key metabolic networks identified through KEGG pathway enrichment. We detected 3,393 metabolites, including 1,844 differentially abundant metabolites: 1,038 between the caput and corpus, 1,243 between the cauda and caput, and 1,159 between the cauda and corpus. KEGG analysis revealed significant enrichment in biosynthesis pathways, cAMP signaling, and protein digestion/absorption. Our findings demonstrate that compartmentalized metabolic reprogramming—particularly involving choline and L-carnitine—drives sperm maturation, providing critical targets for optimizing semen cryopreservation technologies in Hu sheep.
研究领域:
生殖生物学
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代谢组学
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动物科学
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分子生物学
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男科学
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JOURNAL OF CHROMATOGRAPHY A
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2026
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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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ANALYTICA CHIMICA ACTA
·
2023
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IF 6.2
Jie Chen,Pei Zhang,Siyuan Qin,Bei Tan,Siqi Li,Shaoran Tang,Chuyao Liao,Ying Zhang,Zunjian Zhang,Fengguo Xu
The metabolome and lipidome are critical components in illustrating biological processes and pathological mechanisms. Generally, two or more independent methods are required to analyze the two compound panels due to their distinct chemical properties and polarity differences. Here, a novel strategy integrating stepwise solid-phase extraction (SPE) and dansyl chemical derivatization was proposed for all-in-one injection LC-MS/MS analysis of serum metabolome and lipidome. In this workflow, a stepwise elution procedure was firstly optimized to separate the metabolome and lipidome fractions using an Ostro plate. Dansyl chemical derivatization was then applied to label amine/phenol, carboxyl, and carbonyl-containing sub-metabolomes. Our results demonstrated that the dansyl labeling could significantly improve chromatographic separation, enhance the MS response, and overcome the matrix effect of co-eluting lipids . Ultimately, an all-in-one injection LC-MS/MS method measuring 256 lipids (covering 20 subclasses) and 212 metabolites (including amino acids , bile acids , fatty acids , acylcarnitines, indole derivatives, ketones and aldehydes, nucleic acid metabolism, polyamines , etc.) was established. This method was applied to investigate the metabolic changes in cisplatin-induced nephrotoxicity in rats and the results were compared with previous untargeted metabolomics . The presented strategy could predominantly improve the analytical coverage and throughput and can be of great use in discovering reliable potential biomarkers in various applications.
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ANNALS OF MEDICINE
·
2023
·
IF 4.4
Zhengwen Xu,Youran Li,Ying Liu,Shengmin Liu,Lin Zhang,Jing Wang,Shaofei Su,Lin Liu,Lanlan Meng,Hongyuan Zhu,Jingru Sun,Lijun Shao,Lin Li,Yanhong Zhai,Guanghui Li,Zheng Cao
Background As folates are essential for embryonic development and growth, it is necessary to accurately determine the levels of folates in plasma and red blood cells (RBCs) for clinical intervention. The aims of this study were to develop and validate a liquid chromatography-tandem mass spectrometry (LC-MS/MS) method for quantitation of folates in plasma and RBCs and to examine the association between plasma and RBC folate concentrations and gestational diabetes mellitus (GDM), gestational hypertension (GH) and preeclampsia (PE).Methods With the in-house developed LC-MS/MS, a retrospective cross-sectional study was conducted. The healthy pregnant women of first- (n = 147), second- (n = 84) and third-trimester (n = 141) or the women diagnosed with GDM (n = 84), GH (n = 58) or PE (n = 23), that were aged between 22 and 46 years old and registered at our institute, were subjected for measurement of folic acid (FA) and 5-methyltetrahydrofolate (5-MTHF), followed by appropriate statistical association analysis.Results The assay for simultaneous quantitation of FA and 5-MTHF in plasma and RBCs was linear, stable, with imprecision less than 15% and recoveries within ±10%. The lower limits of quantification for FA and 5-MTHF measurement in whole blood were 0.57 and 1.09 nmol/L, and in plasma were 0.5 and 1 nmol/L, respectively. In the association analysis, the patients with lower RBC folate level (<906 nmol/L) presented higher risks of PE development (OR 4.861 [95% CI 1.411–16.505]) by logistic regression and restricted cubic spline (RCS) regression in a nonlinear fashion. In addition, higher level of plasma folates in pregnancy was significantly associated with GH risk but may be protective for the development of GDM.Conclusions The in-house developed LC-MS/MS method for folates and metabolites in plasma or RBC showed satisfactory analytical performance for clinical application. Further, the levels of folates and metabolites were diversely associated with GDM, GH and PE development.
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JOURNAL OF CHROMATOGRAPHY B-ANALYTICAL TECHNOLOGIES IN THE BIOMEDICAL AND LIFE SCIENCES
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2022
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IF 3.318
Yutao Lou,Hui Qin,Qing Hu,Yitao Chai,Hongying Zhou,Mengting Chen,Qiyue Wang,Ping Huang,Jinping Gu,Yiwen Zhang
The objective of this study was to develop and validate a simple, rapid, and sensitive liquid chromatography-tandem mass spectrometry (LC-MS/MS) method for the simultaneous determination of three tyrosine kinase inhibitors (ceritinib, osimertinib, and crizotinib) in human plasma using a single-step protein precipitation extraction. Chromatographic separation was achieved using a Waters X Bridge C18 (2.1 mm × 100 mm, 3.5 µm) and gradient elution with 0.2 % formic acid in water and acetonitrile. The total run time was 4.0 min, and the injection volume was 5 μL. The analytes were detected in the multiple reaction monitoring mode using electrospray ionization with positive ion mode. The m / z transitions of ceritinib, osimertinib, crizotinib and nilotinib were 558.0 → 433.2, 500.0 → 72.1, 450.0 → 259.3, and 530.0 → 289.1, respectively. The method was linear in the range of 2–500 ng/mL with lower limit of quantification of 2 ng/mL. Based on the guidelines on bioanalytical methods by the FDA, the validation studies demonstrated that the three analytes were both precise and accurate at four concentration levels, and the coefficient of variation was < 10.59 % and accuracy was > 88.26 %. We present a simple, rapid, and sensitive method for the simultaneous quantification of ceritinib, osimertinib, and crizotinib in human plasma by LC-MS/MS, which could be used in routine therapeutic drug monitoring.
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JOURNAL OF PHARMACEUTICAL AND BIOMEDICAL ANALYSIS
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2022
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IF 3.571
Dongyuan Lu,Zhipeng Wang,Shouhong Gao,Yuehao Han,Hongsen Wang,Hanglin Li,Hongxia Yan,Bosu Meng,Yuhui Mu,Yi Jiang,Xia Tao,Wansheng Chen
Depression is a mental health disorder characterized by chronic negative mood, and depression has become a major threat to human health and quality of life. Anyupeibo capsule , a fifth-class new Chinese medicine, was prepared with extracts of Piper laetispicum C.DC. (Piperaceae), and the alkaloid K6 (5′-methoxy-3′,4′-methyl-enedioxycinnamic-acidisob-utylamide-isobutylamide) was found to be the main active component. Using high-performance liquid chromatography coupled with triple-quadrupole tandem mass spectrometry (LC-MS/MS), we developed a method to quantify the concentration of K6 in serum samples from patients with depression. Pretreatment of samples was completed based on solid-phase extraction, and the mobile phase for subsequent LC analysis consisted of aqueous ammonium acetate (0.1 mmol/L, phase A) and acetonitrile (phase B) with isocratic elution at 60% B. Chromatographic separation of K6 was achieved within 3 min with an Agilent ZORBAX SB-C 18 column (2.1 × 150 mm, 3.5 µm) at a flow rate of 0.3 mL/min. A linear regression equation for K6 yielded correlation coefficients of r 2 > 0.99 within a linear range 0.0503–100.5000 ng/mL. Extraction recovery ranged from 85.33% to 101.18%, and the matrix effect ranged from 87.15% to 100.28%. The inter-day and intra-day precision values—expressed as relative standard deviation—were less than 15%, and the corresponding accuracy values were within ±15%. All validation results for stability, specificity, and carry-over met the requirements of Pharmacopoeia. The LC-MS/MS method was applied to determine the K6 concentration in serum samples from patients with depression in a phase III clinical trial of Anyupeibo capsule.
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MOLECULES
·
2023
·Vol. 28
·期 10
·4158
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IF 4.6
Yichen Wang,Renjin Zheng,Pingping Wu,Youjia Wu,Lingyi Huang,Liying Huang
Tetrodotoxin (TTX) inhibits neurotransmission in animals, and there is no specific antidote. In clinical practice in China,Althaea rosea(A. roseaflower) extract has been used to treat TTX poisoning. In this work, the efficacy of the ethyl acetate fraction extract ofA. roseaflower in treating TTX poisoning in rats was investigated. A high-performance liquid chromatography–tandem mass spectrometry (LC-MS/MS) method was developed to determine nine neurotransmitters in rat brain tissue, including γ-aminobutyric acid (GABA), dopamine (DA), 5-hydroxytryptamine (5-HT), noradrenaline (NE), 3,4-dihydroxyphenylacetic acid (DOPAC), homovanillic acid (HVA), 5-hydroxyindole-3-acetic acid (5-HIAA), epinephrine (E), and tyramine (Tyn). The detoxifying effect ofA. roseaflower was verified by comparing the changes in neurotransmitters’ content in brain tissue before and after poisoning in rats. The assay was performed in multiple reaction monitoring mode. The quantification method was performed by plotting an internal-standard working curve with good linearity (R2> 0.9941) and sensitivity. Analyte recoveries were 94.04–107.53% (RSD < 4.21%). Results indicated that the levels of 5-HT, DA, E, and NE in the brains of TTX-intoxicated rats decreased, whereas the levels of GABA, Tyn, and 5-HIAA showed an opposite trend, and HVA and DOPAC were not detected. The levels of all seven neurotransmitters returned to normal after the gavage administration of ethyl acetate extract ofA. roseaflower to prove that the ethyl acetate extract ofA. roseaflower had a therapeutic effect on TTX poisoning. The work provided new ideas for studies on TTX detoxification.Keywords:tetrodotoxin;LC-MS/MS;Althaea roseaflower;neurotransmitters;detoxification
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