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.
✓ 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.
✓ 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).
✓ 已验证
产品关联
DOI
PubMed
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
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
·
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.
✓ 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).
✓ 已验证
产品关联
DOI
PubMed
高影响因子
JOURNAL OF PHARMACEUTICAL AND BIOMEDICAL ANALYSIS
·
2023
·
IF 3.4
Mingxia Liu,Jing He,Canjun Ruan,Weigang Pan,Peixian Mao,Zuoli Sun,Gang Wang,Jian Yang
D -amino acids may be indicators of late-life depression but separation and quantification of enantiomers which differ only by optical rotation sign remain challenging due to their identical physical and chemical properties. A convenient LC-MS/MS method was developed for the simultaneous measurement of l - and d -amino acids based on the chiral derivatization reagent, N α -(5-fluoro-2,4-dinitrophenyl)- L -leucinamide, and conventional octadecylsilane reversed-phase column. Methanol was used as the extraction solvent and a single-step derivatization reaction using volatile triethylamine eliminated the requirement for desalination prior to LC-MS/MS. Simultaneous separation and identification of 21 amino acids and the enantiomeric compositions of the 18 chiral proteogenic entities were achieved. Low limits of detection (0.03–4.0 nM), wide linear range (0.01–20 μM), good precision (RSDs < 10 %) and negligible matrix effects indicated the suitability of the method. Application of the method to the quantification of serum chiral amino acids in late-life depression patients (n = 40) and controls (n = 35) found a total of 17 L -amino acids, 14 D -amino acids, D L -asparagine, glycine and γ-aminobutyric acid. The statistical evaluation showed significant differences of glycine, L -threonine and D -methionine between late-life depression patients and controls, indicating that these are potential biomarkers of late-life depression.
✓ 已验证
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).
✓ 已验证
产品关联
DOI
高影响因子
JOURNAL OF PHARMACEUTICAL AND BIOMEDICAL ANALYSIS
·
2025
·
IF 3.1
Xinran Cui,Yongbin Wang,Yan Zhan,Xiaoyan Chen
Dimethoxyethyl phthalate (DMEP) is an industrial phthalates reagent exposed to human body. Its hydrolytic metabolite ethylene glycol methyl ether (EGME) and further oxidative metabolite methoxyacetic acid (MAA) have reproductive and developmental toxicity, and the latter is more toxic than the former. However, due to the lack of sensitive and reliable analytical method, the in vivo clearance and biotransformation of EGME and MAA is poorly understood. In order to evaluate their toxicokinetic profiles, a precolumn derivatization liquid chromatography-tandem mass spectrometry (LC-MS/MS) method was developed and validated for the simultaneous determination of EGME and MAA in rat plasma. After a simple protein precipitation procedure, the sample was derivatized with p -toluene sulfonyl isocyanate (PTSI) and 4-bromo- N -methylbenzylamine (4-BNMA), separated by gradient elution on HSS T3 column, and detected by electrospray ionization (ESI) source in positive multiple reaction monitoring (MRM) mode. The results of the method validation showed that EGME had good linearity in the range of 2.00–400 ng/mL and MAA in the range of 5.00–1000 ng/mL. The intra- and inter-day accuracy and precision were within acceptable limits ( ± 15 %) at all concentrations. This validated method was successfully applied to characterize the toxicokinetics of EGME and MAA in rats following a gavage administration of 50 mg/kg DMEP.
✓ 已验证
产品关联
DOI
PubMed
高影响因子
JOURNAL OF PHARMACEUTICAL AND BIOMEDICAL ANALYSIS
·
2018
·
IF 2.831
Hong Pan,Yi Li,Linyan Huang,Xumei Zhou,Yuanfu Lu,Fuguo Shi
Arecoline is the primary active and toxic constituent of areca nut. Arecaidine and arecoline N -oxide are two major active metabolites of arecoline. In this work, an accurate and simple high performance liquid chromatography tandem mass spectrometry method for simultaneous quantification of arecoline, arecaidine and arecoline N -oxide in rat plasma was developed and fully validated to study their pharmacokinetic behaviors in rats. After extracted from rat plasma by protein precipitation with methanol and then concentrated, the analytes were chromatographic separated on a Sepax Sapphire C 18 analytical column. The mobile phase consisted of methanol and 2 mM ammonium acetate buffer solution containing 0.2% ( v/v ) formic acid (8:92, v/v ) under isocratic elution. The analytes were detected by multiple reaction monitoring (MRM) with an electrospray ionization source in the positive ion mode. The transitions of m / z 156.2 → 53.2, m / z 142.2 → 44.2 and m / z 172.2 → 60.2 were selected for arecoline, arecaidine and arecoline N -oxide, respectively. The method was linear over the concentration range of 0.5–100 ng/mL for arecoline, 5–5000 ng/mL for arecaidine and arecoline N -oxide with no carry-over effect. The accuracies and intra- and inter-batch precisions were all within the acceptance limits. No matrix effect and potential interconversion between the analytes and other metabolites were observed in this method. The validated method was further employed to a preclinical pharmacokinetic study of arecoline, arecaidine and arecoline N -oxide after oral treatment with 20 mg/kg arecoline to rats.
✓ 已验证
产品关联
DOI
PubMed
高影响因子
BIOMEDICAL CHROMATOGRAPHY
·
2013
·Vol. 28
·期 7
·994-1002
·
IF 1.945
Ting Zhou,Ting Zhao,Qing Cheng,Shan Liu,Ling Xu,Wen Tan
A sensitive liquid chromatography–tandem mass spectrometry (LC-MS/MS) method for simultaneous determination of R -bambuterol and its active metabolite R -terbutaline in human plasma and urine was established. The inhibition for the biotransformation of R -bambuterol in plasma was fully investigated. Plasma samples were prepared on ice and neostigmine metilsulfate added as a cholinesterase inhibitor immediately after sample collection. All samples were extracted with ethyl acetate and separated on a C 18 column under gradient elution with a mobile phase consisting of methanol and water containing 5 m m ammonium acetate at a flow rate of 0.6 mL/min. The analytes were detected by an API 4000 tandem mass spectrometer with positive electrospray ionization in multiple reaction monitoring mode. The established method was highly sensitive with the lower limit of quantification (LLOQ) of 10.00 pg/mL for each analyte in plasma. In urine samples, the LLOQs were 20.00 and 500.0 pg/mL for R -bambuterol and R -terbutaline, respectively. The intra- and inter-day precisions were <12.7 and <8.6% for plasma and urine, respectively. The analytical runtime within 6.0 min per sample made this method suitable for high-throughput determination. The validated method has been successfully applied to the human pharmacokinetic study of R -bambuterol involving 10 healthy volunteers. Copyright © 2013 John Wiley & Sons, Ltd.
✓ 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）