Frontiers in Veterinary Science
·
2023
·
IF 3.2
Shiting Xie,Yixing Lu,Jun Wang,Changcheng Lin,Peiyu Ye,Xiaolin Liu,Wenguang Xiong,Zhenling Zeng,Dongping Zeng
Introduction Milbemycin oxime (MBO) and praziquantel (PZQ) have a broad spectrum of biological activity and are commonly used to treat the parasitic infection in the veterinary clinic. In this study, a fast and efficient LC-MS/MS method was established and validated for the simultaneous determination of MBO, PZQ, cis-4-hydroxylated-PZQ (C-4-OH-PZQ) and trans-4-hydroxylated-PZQ (T-4-OH-PZQ) and in cat plasma. Methods Extraction of analytes and internal standards from cat plasma by acetonitrile protein precipitation, allows rapid processing of large batches of samples. MBO, PZQ, C-4-OH-PZQ, T-4-OH-PZQ, and internal standard (IS) were eluted for 13.5 min on a C 18 column with a 0.1% formic acid water/acetonitrile mixture as the mobile phase. Results Results showed that the method had good precision, accuracy, recovery, and linearity. The linearity range was 2.5–250 ng/mL for MBO, and 10–1000 ng/mL for PZQ, C-4-OH-PZQ, and T-4-OH-PZQ. The intra-day and inter-day precision CV values of the tested components were within 15%. The extraction recoveries of the four components ranged from 98.09% to 107.46%. The analytes in plasma remained stable for 6 h at room temperature, 26 h in the autosampler (4 °C), after freeze–thaw (−20°C) cycles, and 60 days in a −20°C freezer. Method sensitivity sufficed for assessing pharmacokinetic parameters of MBO, PZQ, C-4-OH-PZQ, and T-4-OH-PZQ in plasma samples with LLOQ of 2.5 ng/mL for MBO and 10 ng/mL for PZQ, C-4-OH-PZQ, and T-4-OH-PZQ. Conclusion In this study, a selective and sensitive LC-MS/MS method for the simultaneous quantification of MBO, PZQ, C-4-OH-PZQ, and T-4-OH-PZQ in cat plasma was developed and validated.This method had been successfully applied to evaluate the pharmacokinetics of MBO, PZQ, C-4-OH-PZQ, and T-4-OH-PZQ after a single oral administration of 8 mg MBO and 20 mg PZQ in cats.
研究领域:
兽医学
·
分析化学
·
药理学
✓ 已验证
产品关联
DOI
PubMed
高影响因子
JOURNAL OF PHARMACEUTICAL AND BIOMEDICAL ANALYSIS
·
2014
·
IF 2.829
Feng Chen,Hai-Long Li,Yin-Feng Tan,Yong-Hui Li,Wei-Yong Lai,Wei-Wei Guan,Jun-Qing Zhang,Yuan-Sheng Zhao,Zhen-Miao Qin
Alpinia oxyphylla (Yizhi) capsularfruits are commonly used in traditional medicine. Pharmacological studies have demonstrated that A. oxyphylla capsularfruits have some beneficial roles. Besides volatile oil, sesquiterpenes, diarylheptanoids and flavonoids are main bioactive constituents occurring in the Yizhi capsularfruits. The representative constituents include tectochrysin, izalpinin, chrysin, apigenin-4′,7-dimethylether, kaempferide, yakuchinone A, yakuchinone B, oxyphyllacinol and nootkatone. Their content levels in the fruit and its pharmaceutical preparations have been reported by our group. The nine phytochemicals are also the major components present in the Yizhi alcoholic extracts, which have anti-diarrheal activities. However, the fates of these constituents in the body after oral or intravenous administration remain largely unknown. In the present study, we focus on these phytochemicals albeit other concomitant compounds. The chemicals and their metabolites in rat plasma were identified using liquid chromatography/tandem mass spectrometry with selected reaction monitoring mode after orally administered Yizhi extract to rats. Rat plasma samples were treated by methanol precipitation, acidic or enzymatic hydrolysis. This target analysis study revealed that: (1) low or trace plasma levels of parent chemicals were measured after p.o. administration of Yizhi extract, Suoquan capsules and pills to rats; (2) flavonoids and diarylheptanoids formed mainly monoglucuronide metabolites; however, diglucuronide metabolites for chrysin, izalpinin and kaempferide were also detected; (3) metabolic reduction of Yizhi diarylheptanoids occurred in rats. Yakuchinone B was reduced to yakuchinone A and then to oxyphyllacinol in a stepwise manner and subsequently glucuronidated by UDP-glucuronosyl transferase. Further research is needed to characterize the UDP-glucuronosyl transferase and reductase involved in the biotransformation of Yizhi chemicals.
研究领域:
药理学
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分析化学
✓ 已验证
DOI
高影响因子
Analytical Methods
·
2016
·Vol. 8
·期 9
·2069-2081
·
IF 1.915
Qi Wen,Hai-Long Li,Yin-Feng Tan,Xu-Guang Zhang,Zhen-Miao Qin,Wei Li,Yong-Hui Li,Jun-Qing Zhang,Feng Chen
Alpiniae oxyphyllae Fructus (Yizhi in Chinese) is commonly used for the treatment of diarrhea, intestinal disorders and urinary incontinence symptoms. To date, little information is available on the pharmacokinetic (PK) properties of this herb. We have identified the known active chemicals (including nootkatone, yakuchinone A, yakuchinone B, oxyphyllacinol, tectochrysin, chrysin, izalpinin, apigenin-4′,7-dimethylether, and kaempferide) and their metabolites (phase II metabolites and oxidized product such as kaempferol) from Yizhi extract in rat plasma using liquid chromatography/tandem mass spectrometry (LC-MS/MS) with selected reaction monitoring. In the present study, an LC-MS/MS-based method was developed and validated for the simultaneous quantitation of the Yizhi chemicals and their metabolites in rat plasma after enzymatic treatment. A mixture of β-glucuronidase and sulfatase was used to liberate parent chemicals from their phase II metabolites. A post-extraction spike method, as well as a post-column infusion method, was conducted to investigate matrix-effects. Particularly, the ion suppression effect for all the analytes was overcome through combining a liquid–liquid extraction method for clean-up, elution gradient optimization for separation and inclusion of very low concentration of HCOOH into the mobile phase. Mean accuracies were obtained in the range of 84.7–112% at three different quality control levels for the ten analytes, with intra- and inter-day variations within 13.6% (1.76–13.6%). This validated method was successfully applied to a PK investigation in rats after a single oral administration of Yizhi extract. These results supply a suitable reference for further PK studies of the Yizhi chemicals and their metabolites in the future.
研究领域:
中药学
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分析化学
·
药理学
✓ 已验证
DOI
高影响因子
JOURNAL OF PHARMACEUTICAL AND BIOMEDICAL ANALYSIS
·
2026
·
IF 3.4
Hui Yan,Haoyang Lu,Shanqing Huang,Yuqing Li,Hui Xia,Wanting Huang,Dewei Shang,Ming Zhang
Dysregulation of the tryptophan (TRP) metabolic pathway is closely linked to the pathophysiology of neuropsychiatric disorders, such as depression. This study aimed to develop and validate a sensitive, rapid, and robust liquid chromatography-tandem mass spectrometry (LC-MS/MS) method for the simultaneous quantification of TRP and its metabolites, kynurenine (KYN) and kynurenic acid (KYNA), in human serum. Analytes were extracted from 100 µL of serum via simple protein precipitation with acetonitrile. Chromatographic separation was achieved on an Agilent ZORBAX HILIC Plus column (4.6 mm×100 mm, 3.5 µm) using isocratic elution with a mobile phase of methanol: acetonitrile containing 5 mM ammonium formate. Quantification was performed using an electrospray ionization source in positive ion multiple reaction monitoring (MRM) mode, with a total run time of only 2.0 min.The linear ranges were 1- 50 µg/mL for TRP, 0.1-5 µg/mL for KYN, and 1-50 ng/mL for KYNA, covering clinically relevant levels. A weighting factor of 1/x² provided the best fit for calibration curves (R² > 0.99). Extraction recoveries ranged from 88.23% to 99.39%, and mean internal standard-normalized matrix effects were 81%-100%. Accuracy and precision values met bioanalytical acceptance criteria. Stability assessments confirmed that samples were stable at -20°C and -80°C for 31 days and through three freeze-thaw cycles. This validated method was successfully applied to analyze serum samples from 103 adolescent patients with first-episode depression.
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产品关联
DOI
PubMed
高影响因子
JOURNAL OF SEPARATION SCIENCE
·
2021
·Vol. 44
·期 7
·1391-1403
·
IF 3.645
Ning Wang,Yue-Wu Xie,Meng-Yu Li,Fei-Fei Li,Li-Yuan Zhang,Yu-Lin You,Shu-Qi Wang
Rauvolfia vomitoria is widely distributed in the tropical regions of Africa and Asia, and has been used in traditional folk medicine in China. Indole alkaloids were found to be major bioactive components, while the effects of diabetes mellitus on the pharmacokinetic parameters of the components have not been reflected in vivo. In this study, an efficient and sensitive liquid chromatography–tandem mass spectrometry method was developed and validated for the simultaneous determination of five ingredients of R. vomitoria in rats. Detection was implemented in multiple-reaction-monitoring mode with an electrospray positive-ionization source. Validation parameters were all in accordance with the current criterion. The established method was effectively employed to compare the pharmacokinetic behaviors of five alkaloids (reserpine, yohimbine, ajmaline, ajmalicine, and serpentine) between normal and type 2 diabetic rats. The single-dose pharmacokinetic parameters of the five alkaloids were determined in normal and diabetic rats after oral administration of 100 and 200 mg/kg body weight. The results indicated that diabetes mellitus significantly altered the pharmacokinetic characteristics of yohimbine, ajmaline, and ajmalicine after oral administration in rats. This is an attempt to provide some evidence for clinicians that may serve as a guide for the use of antidiabetic medicine in clinical practice.
研究领域:
药理学
·
分析化学
✓ 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
·
2018
·
IF 2.441
Lihan Sun,Huajing Wu,Lianjie Ren,Jiaojiao Cong,Xiaohui Qin,Xingli Wang,Xinming Qi,Lifeng Kang,Junying Zhang,Chunyong Wu
A sensitive and specific liquid chromatography coupled with tandem mass spectrometry (LC-MS/MS) method was developed and validated for quantitative analysis of 1,2:5,6-dianhydrogalactitol (DAG) in mouse plasma and tissues. Sodium diethyldithiocarbamate (DDTC) was used as the derivatization reagent to improve its LC-MS/MS behavior. Analytes were separated on a Welch Ultimate XB-CN column with a mobile phase consisting of acetonitrile and 0.1% formic acid solution (65:35). The MS analysis was conducted by positive electrospray ionization in multiple-reaction monitoring (MRM) mode. Good linearity (r 2 > 0.9958) was observed over the concentration range of 1–1000 ng/mL in plasma and tissue homogenates (brain, liver, heart, spleen, lung and kidney). The intra- and inter-batch precision and accuracy of DAG in plasma and brain samples were all within the acceptable limits. The extraction recovery was stable and no significant matrix effects were observed. The method was successfully applied to study the pharmacokinetic and tissue distribution of DAG in mice after intravenous administration. DAG could cross the blood-brain barrier and had limited liver distribution. Rat primary hepatocytes in vitro experiments demonstrated that DAG had a safe profile in liver.
研究领域:
药物分析
·
药理学
✓ 已验证
产品关联
DOI
PubMed
高影响因子
BIOMEDICAL CHROMATOGRAPHY
·
2025
·Vol. 39
·期 2
·e6063
·
IF 1.7
Fan Tang,Xiaoli Hou,Jiajie Chen,Yasen Cao,Yixia Wang,Hong Cheng
Mobocertinib is a potent selective tyrosine kinase inhibitor approved for the treatment of non–small cell lung cancer with activating EGFR exon 20 insertions. The aim of this study was to develop a procedure for liquid chromatography tandem mass spectrometry (LC-MS/MS) for the determination of mobocertinib and its metabolite desmethyl-mobocertinib in human plasma. The human plasma samples were precipitated with acetonitrile and analyzed using a Waters ACQUITY BEH C 18 column coupled to a 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. Mobocertinib and desmethyl-mobocertinib were monitored by multiple reaction monitoring (MRM) with m / z 586.5 > 72.2 and 572.4 > 473.2, respectively. The procedure demonstrated excellent linearity ( r > 0.997) within the concentration range of 0.1–200 ng/mL for both analytes. Precision in relative standard deviation was < 9.37% for mobocertinib and < 12.03% for desmethyl-mobocertinib. Accuracy in relative error was within −7.23% to 9.18% for mobocertinib and −2.78% to 9.87% for desmethyl-mobocertinib. Extraction recovery was > 80% for both analytes. The validated LC-MS/MS method was successfully applied to the pharmacokinetic study of mobocertinib and desmethyl-mobocertinib in healthy human volunteers with K 2 EDTA as anticoagulant after a single dose of mobocertinib (160 mg).
研究领域:
药理学
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分析化学
·
肿瘤学
✓ 已验证
产品关联
DOI
PubMed
高影响因子
CHEMICAL ENGINEERING JOURNAL
·
2026
·
IF 12.5
Yanmei Shi,Liqin Chao,Xiaobing Liu,Zhihong Chen,Zhenghui Chang,Sisen Zhang,Shusheng Zhang,Kai Hu
Development of advanced in vivo sampling tools for the synchronous monitoring of drugs and endogenous biomarkers is critical for integrated pharmacokinetic-pharmacodynamic (PK-PD) studies. Herein, a novel solid-phase microextraction (SPME) fiber coating was engineered based on a zwitterionic covalent organic framework (EB-TTB-DABSA COF), strategically functionalized with sulfonate and quaternary ammonium groups. This rationally designed coating provides synergistic electrostatic, π–π, and hydrophobic interactions, enabling the efficient and simultaneous extraction of both cationic alkaloids and neurotransmitters. Coupled with LC-MS/MS, the developed platform achieved highly sensitive (limits of detection down to 3.3 × 10 −3 ng·mL −1 ), minimally invasive, and synchronous monitoring of these analytes in paired blood and brain matrices of living rats. Application in a Parkinson's disease (PSD) model revealed altered pharmacokinetics of Coptis chinensis alkaloids, including significantly increased area under the curve (AUC) values ( p < 0.01) and prolonged elimination half-lives compared to controls. These findings indicate enhanced systemic absorption and improved bioavailability of alkaloids under PSD conditions. Crucially, pharmacodynamic analysis showed that alkaloid administration triggered a synchronized restoration of key depleted neurotransmitters in PSD brains. A correlation with a characteristic hysteresis pattern further established a delayed neuroprotective relationship between alkaloid concentrations and neurotransmitter levels. This study not only introduces a robust zwitterionic COF-SPME platform for concurrent in vivo biosampling but also provides the first quantitative neuropharmacological perspective on Coptis chinensis alkaloids, offering a foundational framework for mechanistic research and therapeutic development in PSD.
✓ 已验证
DOI
高影响因子
FOOD CHEMISTRY
·
2026
·
IF 9.8
Yawen He,Chengxun Lin,Bin Zhang,Zixuan Wang,Jiangui Li,Zhenfan Yu
Fuji apples from the Aksu production region are highly favored by consumers. In contrast, those from the Yili region exhibit marked differences in flavor profiles, the mechanisms of which remain unclear. This study investigated the flavor variations in Fuji apples from these two producing regions by integrating analyses of both volatile and non-volatile metabolites. The results from the electronic nose and electronic tongue indicated that the sensors for W1W, W2W, W5S, and sourness exhibited the most pronounced responses in Fuji apples from the Aksu region. 16 key aroma-active compounds and 143 non-volatile differential compounds were identified. The aroma of Fuji apples was predominantly characterized by esters and terpenoids, with representative compounds including hexyl 2-methylbutanoate, 3-Methylbutyl acetate, 2-Methylbutyl acetate, and citronellol. These compounds collectively impart fruity, sweet, and floral notes. Furthermore, the peel of the ‘Yanfu 6’ cultivar from Aksu exhibited distinctive rosy and woody notes, while its pulp possessed a pineapple-like aroma. KEGG pathway enrichment analysis demonstrated that amino acid metabolism, fatty acid metabolism, and phenylalanine metabolism are interconnected. This study provides valuable insights for systematically understanding the formation of characteristic aromas in Fuji apples from the Xinjiang region
✓ 已验证
产品关联
DOI
PubMed
高影响因子
ANALYTICAL AND BIOANALYTICAL CHEMISTRY
·
2021
·Vol. 413
·期 7
·1799-1807
·
IF 4.157
Ouyang Zhonghua,Huang Jing,Ren Yi,Li Huanhuan,Ding Yao,Zhang Ke,Jiang Lei,Yu Peng
High-dose methotrexate (HDMTX) combined with leucovorin (LV) is the first-line drug therapy for many kinds of malignant tumors. However, the specific treatment plans, such as dosage and duration of administration, are usually formulated according to the clinician’s experience and therapeutic drug monitoring (TDM) of methotrexate in patients’ plasma, which are responsible for strong individual differences of drug usage. A large number of studies have shown that methotrexate targets the inside of the cell. The key cytotoxic component is the methotrexate polyglutamates (MTXPGs) in the cell. The concentration of methotrexate in plasma does not reflect the efficacy and side effects well. Based on mass spectrometry technology, we developed and validated an accurate, sensitive, and stable method to quantify the intracellular MTX (MTXPG 1 ) and its metabolites MTXPG 2–7 simultaneously. The lower limit of quantification was 0.100 ng/ml, and the run time was only 3 min. Moreover, our team has already developed two LC-MS/MS-based methods to respectively quantify methotrexate in plasma samples and two key proteins (γ-glutamyl hydrolase [GGH] and folylpolyglutamate synthetase [FPGS]) in peripheral blood mononuclear cells (PBMC). Through these highly sensitive and accurate approaches, we have gained a deep understanding of the whole pharmacokinetic process of MTX and explored the key factors affecting the accumulation process of intracellular active components (MTXPGs). Based on this research, it is possible to find a more effective way to provide an accurate reference for clinical drug use than traditional therapeutic drug monitoring (TDM).
研究领域:
药理学
·
临床化学
·
肿瘤学
·
分析化学
·
药学
✓ 已验证
产品关联
DOI
PubMed
高影响因子
Analytical Methods
·
2018
·Vol. 11
·期 4
·507-516
·
IF 2.073
Chang Liu,Diandian Deng,Di Xu,Kang Wu,Hong Yang,Kang Zhao,Jianguo Li,Anping Deng
In this study, a monoclonal antibody (mAb)-based enzyme-linked immunosorbent assay (ELISA) for the determination of chloramphenicol (CAP) in shrimp, feed and milk samples was developed and validated by LC-MS/MS coupled with immunoaffinity clean-up (LC-MS/MS-IAC). Three immunogens were synthesized and used to immunize mice. Spleen cells from the immunized mice with the highest titer were selected for cell fusion. Two lines of hybridoma cells (1B1 and 2D2) secreting specific antibodies against CAP were successfully screened. Under optimal conditions, the values of the 50% inhibitory concentration (IC50) and limit of detection (LOD) of the ELISA in phosphate-buffered saline (PBS) based on 2D2 mAb for the detection of CAP were 0.46 ng mL−1 and 0.06 ng mL−1, respectively. There was no cross-reactivity (CR) of the ELISA with other antibiotics (florfenicol, thiamphenicol, etc.). Shrimp, feed and milk samples were spiked with different contents of CAP and detected by ELISA. The recoveries and coefficients of variation (CVs) of the ELISA for CAP from three spiked samples were 80.6–116.0% and 5.5–15.4% (n = 3), 96.2–111.0% and 7.0–13.5% (n = 3), and 79.7–109.8% and 5.8–13.3% (n = 3), respectively. As the CAP concentrations in spiked samples measured by LC-MS/MS coupled with solid phase extraction (LC-MS/MS-SPE) were significantly lower than those measured by ELISA, we established an immunoaffinity clean-up (IAC) for CAP by covalently immobilizing our mAb against CAP on the CNBr-activated Sepharose-4B gel and directly mixing the mAb-immobilized gel with the spiked samples sufficiently. The recoveries of CAP from the spiked samples measured by LC-MS/MS-IAC were 78.6–106.7% with the CV less than 11.1% (n = 3).
研究领域:
分析化学
·
食品科学
·
兽医学
✓ 已验证
产品关联
DOI
高影响因子
FOOD CHEMISTRY
·
2022
·
IF 9.231
Xiaoli Guo,Tingze Ren,Jianchun Ji,Yan Yang,Xin Di
In this work, a combination of QuEChERS and dispersive micro-solid phase extraction (D-μ-SPE) based on dissolvable layered double hydroxide (LDH) has been established for preconcentration and enrichment of sulfonylurea herbicides (SUHs) in wolfberry samples. The QuEChERS was used for extraction and purification of SUHs, followed by D-μ-SPE for further enrichment of targeted analytes to obtain superior extraction performance. Dissolvable LDH nanosheets were used as absorbents, thus eliminating the elution step needed in traditional D-μ-SPE. The main influence experimental variables including pH of sample solution, amount of LDH, vortex time and volume of acidic solution were optimized in detail. Under the optimized conditions, the proposed method shows high precision (RSDs < 12 .7%), low limits of detection (0.01–0.5 ng/g) and limits of quantitation (0.1–2.0 ng/g), acceptable recovery (80.1%–97.1%), thus making it a good alternative analytical strategy for the determination of SUHs residues at the low nanogram per gram range with desirable sensitivity.
研究领域:
分析化学
·
环境科学
·
食品科学
✓ 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）