ANALYTICAL AND BIOANALYTICAL CHEMISTRY
·
2019
·Vol. 411
·期 15
·3361-3372
·
IF 3.286
Zhang Yingyi,Li Liang,Wang Qi,Shen Mei,Han Weili,Yang Xuemei,Chen Lingyun,Ma Ande,Zhou Zhengzheng
Methamphetamine (METH) is one of the most highly addictive illicit drugs abused all over the world. Much evidence indicates that METH abuse leads to major toxicity, medical consequences, and even severe public health consequences. Existing studies usually focus on the pathomechanism of METH-induced toxicity; therefore, data on metabolites and elements correlating with particular toxicity remain scarce. The objective of the present study is to develop appropriate analytical procedures to identify the differential metabolic and elemental biomarkers on METH-induced hepatic injury to rats. The rats were administrated with METH (15 mg/mL/kg, two times per day) via intraperitoneal (i.p.) injections for four consecutive days. The alanine aminotransferase and aspartate aminotransferase activity levels of in the rat serum of the METH group increase significantly compared with those of the control group, suggesting obvious hepatic injury. The results are further confirmed by the histopathological microscopic observation. A total of 18 small molecular metabolites and 19 elements are selected to perform the simultaneous quantification based on the combination of liquid chromatography coupled with tandem mass spectrometry and inductively coupled plasma mass spectrometry. Sample preparation was optimized to cover all the analytes. Both methods are optimized and validated according to developed guidelines such as limits of detection, limits of quantification, linearity, precision, and recovery. All the obtained data are within the satisfactory range. The normalized data were processed according to the partial least squares discrimination analysis (PLS-DA) model. Five differential metabolic and six elemental markers are identified in rat plasma based on the variable importance in projection (VIP) (> 1) and t test results. Overall, the results obtained in this study demonstrate the developed methods are suitable for simultaneous determination of metabolic and elemental markers in the hepatic injury to rats induced by METH.
Graphical abstract
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JOURNAL OF PHARMACEUTICAL AND BIOMEDICAL ANALYSIS
·
2019
·
IF 2.983
Shuai Ji,Xian Shao,Zhen-yu Su,Lei Ji,Yu-jie Wang,Yun-su Ma,Lu Zhao,Yan Du,Meng-zhe Guo,Dao-quan Tang
Fufang Danshen Dripping Pill (FDDP) and Clopidogrel Bisulfate Tablet (CBT) are usually combined for treatment of coronary artery diseases in clinical. To investigate the pharmacokinetic interaction between FDDP and CBT after oral administration of FDDP, CBT and their combination in rats, a novel LC–MS method with segmented scan modes (multiple reaction monitoring and selected ion monitoring) and polarity (positive and negative ionization) was developed. Clopidogrel and the main active ingredients of FDDP, with different chemical and ionization properties, were simultaneously quantified in plasma in a single run. The method was validated in terms of specificity, linearity, precision, accuracy, recovery, matrix effect and stability. As a result, co-administration of FDDP and CBT significantly altered the pharmacokinetic parameters of danshensu, ginsenoside Rb1, dihydrotanshinone I, tanshinone I and tanshinone IIA of FDDP, as well as clopidogrel. Mechanism studies suggested that induction of liver cytochrome P450 isozymes CYP2C11 and CYP3A1 by co-administration, as well as inhibition of carboxyl esterase 1, was partly responsible for FDDP-CBT pharmacokinetic interactions. The developed LC–MS method could be used to simultaneously quantify different types of in vivo analytes in a single run, and the results could be used for clinical medication guidance of FDDP and CBT.
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ANALYTICAL AND BIOANALYTICAL CHEMISTRY
·
2018
·Vol. 410
·期 7
·2011-2018
·
IF 3.307
Yu Lingling,Wen Chao,Li Xing,Fang Shiqi,Yang Lichuan,Wang Tony,Hu Kaifeng
Quantification of endogenous and exogenous plasma glucose can help more comprehensively evaluate the glucose metabolic status. A ratio-based approach using isotope dilution liquid chromatography tandem mass spectrometry (ID LC-MS/MS) with indirect multiple reaction monitoring (MRM) of the derivative tag was developed to simultaneously quantify endo-/exogenous plasma glucose. Using diluted D-[ 13 C 6 ] glucose as tracer of exogenous glucose, 12 C 6 / 13 C 6 glucoses were first derivatized and then data were acquired in MRM mode. The metabolism of exogenous glucose can be tracked and the concentration ratio of endo/exo-genous glucose can be measured by calculating the endo-/exo-genous glucose concentrations from peak area ratio of specific daughter ions. Joint application of selective derivatization and MRM analysis not only improves the sensitivity but also minimizes the interference from the background of plasma, which warrants the accuracy and reproducibility. Good agreement between the theoretical and calculated concentration ratios was obtained with a linear correlation coefficient ( R ) of 0.9969 in the range of D-glucose from 0.5 to 20.0 mM, which covers the healthy and diabetic physiological scenarios. Satisfactory reproducibility was obtained by evaluation of the intra- and inter-day precisions with relative standard deviations (RSDs) less than 5.16%, and relative recoveries of 85.96 to 95.92% were obtained at low, medium, and high concentration, respectively. The method was successfully applied to simultaneous determination of the endo-/exogenous glucose concentration in plasma of non-diabetic and type II diabetic cynomolgus monkeys.
Graphical Abstract The scheme of the proposed ratio-based approach using isotope dilution LC-MS/MS with indirect MRM of the derivative tag for simultaneous quantification of endogenous and exogenous plasma glucose.
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JOURNAL OF PHARMACEUTICAL AND BIOMEDICAL ANALYSIS
·
2022
·
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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JOURNAL OF CHROMATOGRAPHY B-ANALYTICAL TECHNOLOGIES IN THE BIOMEDICAL AND LIFE SCIENCES
·
2022
·
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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Frontiers in Environmental Science
·
2021
·
IF 4.581
Jin Hui,Zhao Cheng,Yin Yi,Zheng Guangming,li Lichun,Shan Qi,Zhang Meiyu,Wei Linting,Shi Xiaona,Huang Heqing,Zhang Wenjing,Liu Shugui
A simple, sensitive, and simultaneous method was established and validated for the active clinical components of teicoplanin and ramoplanin in environmental water by LC-MS/MS coupled with cascade elution. Moreover, a cascade elution method, which was rapid, solvent-less, and high-extraction efficient was successfully proposed to realize the extraction and purification of seven targets in one step. Under optimized conditions, the method showed excellent linearity with the correlation coefficient (R2) ≥0.998 in the range of 1.0–100.0 ng L−1. Low matrix effects and good recoveries which ranged from 86 to 114% were reached with RSDs lower than 3.0% for most targets. The limits of detection and limit of quantification were 0.1–1.3 and 0.3–4.0 ng L−1, respectively. This method was successfully applied for the determination of teicoplanin and ramoplanin in water samples from the Pearl River and the South China Sea. TA2-2,3 was quantified in only one sample with the concentration of 8.0 ng L−1.
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MOLECULES
·
2021
·Vol. 26
·期 8
·2327
·
IF 4.412
Yuanyuan Liu,Yanfang Yang,Bangyuan Wang,Renyun Wang,Jianmei Pang,Yu Jiang,Yuling Liu
Houttuynia essential oil (HEO) has excellent antiviral, anti-inflammatory, and other pharmacological effects, but the lack of effective analytical methods to quantify HEO in plasma has hindered its better clinical monitoring. Houttuynine (Hou) is one of the main active ingredients and quality control substances of HEO, so the pharmacokinetic study of HEO could be conducted by determining Hou blood concentration. Hou is active and not stable in plasma, which makes its blood concentration difficult to measure. In this work, a novel liquid chromatography tandem mass spectrometry (LC-MS/MS) method for Hou determination in rat blood was established that involves Hou being derivatized with 2, 4-dinitrophenylhydrazine to form a stable compound to prevent degradation. Herein,p-Tolualdehyde-2,4-dinitrophenylphenylhydrazone was selected as an internal standard substance and the LC-MS/MS method was evaluated for selectivity, precision, accuracy, calibration limit, matrix effect, recovery, and stability. Good linearity (r2= 0.998) was reached in the range of 2–2000 ng/mL, and the lower limit of quantification of Hou was determined to be 2 ng/mL. The mean intra-assay accuracy ranged from 77.7% to 115.6%, whereas the intra-assay precision (relative standard deviation, RSD) was below 11.42%. The matrix effect value for Hou in rat plasma was greater than 75%, and for the internal standard (IS) it was 104.56% ± 3.62%. The extraction recovery of Hou were no less than 90%, and for the IS it was 96.50% ± 4.68%. Our method is sensitive and reliable and has been successfully applied to the pharmacokinetic analysis of Hou in rats given HEO via gavage and injection.Keywords:Houttuynia cordataThunb.;houttuynine;houttuynia essential oil;LC-MS/MS;pharmacokinetic study
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BIOMEDICAL CHROMATOGRAPHY
·
2021
·Vol. 35
·期 6
·e5076
·
IF 1.902
Kaiyang Wang,Lan Luo,Xiaoli Xu,Xingyu Chen,Qiong He,Zhongjie Zou,Shumei Wang,Shengwang Liang
Dyspepsia, one of the most prevalent diseases of the digestive tract that impacts the quality of patient life, is mainly caused by gastrointestinal motility disorder. Hawthorn is a commonly used traditional Chinese medicine for treating dyspepsia, and has been proven to improve gastrointestinal motility. Herein, a rat model of gastrointestinal motility disorder was established by subcutaneous injection with atropine. The modeled rats were treated with four polar parts (T1–4 in descending polarity, corresponding to water, n -butanol, ethyl acetate and petroleum ether extracts, respectively) of hawthorn. Through metabolomics analysis, a total of 20 significantly metabolites were identified with significant changes in their abundance levels and these metabolites were related to many metabolic pathways such as amino acid metabolism and primary bile acid biosynthesis. The results showed that T3 had the best therapeutic effect of promoting gastrointestinal motility. Other parts showed no obvious therapeutic effect, demonstrating that the effective components of hawthorn may be compounds of medium polarity. T3 might achieve good therapeutic effects owing to the gastrointestinal motility promotion activity, and by rectifying the disturbed metabolic pathways in the gastrointestinal motility disorder model.
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MICROCHIMICA ACTA
·
2020
·Vol. 187
·期 7
·1-8
·
IF 6.232
Li Nianlu,Li Ruohan,Song Yinshuang,Ma Long,Gao Cuiling,Li Lili,Cheng Shi-Bo,Zhang Xiaoli,Chen Jing,Zhan Jinhua
Carbonaceous shell-coated γ-Fe 2 O 3 nanoparticles (γ-Fe 2 O 3 @CNM) were synthesized from glucose caramelization and used as a novel magnetic solid-phase extraction medium for malachite green and crystal violet in environmental water. Malachite green and crystal violet were absorbed on to γ-Fe 2 O 3 @CNM by electrostatic and π-interactions. The morphologies, pore structures, surface functional groups, and magnetic properties of γ-Fe 2 O 3 @CNM were characterized by TEM, FTIR, hysteresis regression, Brunauer-Emmet-Teller analysis, zeta potential, XPS, and XRD. The magnetic solid-phase extraction procedure was optimized by extraction pH, absorption time, desorption solvent, and desorption time. The absorption capacities (q max values) for malachite green and crystal violet were 34.2 and 27.9 mg g −1 , respectively. After magnetic solid-phase extraction, malachite green and crystal violet were determined by LC-MS/MS. The analytical method was validated with a linear range of 0.02–20 ng mL −1 , enrichment factor of 25.8 and 25.4, method detection limit of 0.004 ng mL −1 , and intra-day precisions of 2.1% and 2.6% for malachite green and crystal violet, respectively. The relative recovery was found to be 73.4–101.5% for malachite green and 83.1–102.7% for crystal violet upon the application of the magnetic solid-phase extraction method to real water samples from lake, spring, sea, fishpond, and industrial waste.
Caramelized-carbon-coated magnetic nanoparticles are used as novel extraction medium based on electrostatic and π-interactions. It is porous, amphiphilic, electronegative, magnetically strong, and features abundant absorption site. These characteristics stimulate mass transfer and result in a useful MSPE method in environmental analysis.
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JOURNAL OF PHARMACEUTICAL AND BIOMEDICAL ANALYSIS
·
2020
·
IF 3.209
Xiangling Feng,Yan Cao,Yufeng Ding,Heng Zheng
Topiroxostat is a recently identified safe and selective xanthine oxidoreductase inhibitor and has been used as a urate-lowing agent for the treatment of hyperuricemia and gout in Japan. In this study, we developed a sensitive, selective and high-throughput method that determines topiroxostat in human plasma using high-performance liquid chromatography-tandem mass spectrometry (HPLC–MS/MS) and it was firstly validated. The samples were prepared by protein precipitation with acetonitrile and dilution of the supernatant in water. The chromatographic separation was conducted on an ACE Excel 5 C18-PFP column (2.1 × 50.0 mm) with gradient elution using a mixture of buffer (2 mM ammonium acetate in 0.1 % formic acid) and acetonitrile as the mobile phase at a flow rate of 0.45 mL/min. The total run time lasted 4.0 min. Tandem mass spectrometry, was performed in positive ionization and multiple reaction monitoring (MRM) modes, with the transitions of m/z 249.2→221.1 for topiroxostat and m/z 253.2→225.1 for topiroxostat-d 4 , respectively. The method was validated and the selectivity, carry-over effect, linearity, accuracy, precision, extraction recovery, matrix effect, and stability were acceptable according to the US Food and Drug Administration and the European Medicines Agency regulations. The method was successfully applied to a clinico-pharmacokinetic study involving twelve healthy Chinese subjects under fasting condition.
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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.
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Analytical Methods
·
2014
·Vol. 6
·期 21
·8675-8681
·
IF 1.938
Waner Hou,Guanghui Liu,Xiuman Sun,Zhiyong Xie,Rongbiao Pi,Wei He,Manna Lin,Qiongfeng Liao
The aim of the present work was to develop and validate an LC-MS/MS method with electrospray ionization (ESI) for the quantification of lipoic acid–fasudil dimer (L–F 001), a novel multi-functional neuroprotective drug in rat plasma, using tetrahydropalmatine as an internal standard. The separation was carried out on a C18 column using a mobile phase consisting of acetonitrile and water (containing 5 mmol l−1 ammonium acetate adjusted to pH 5.0 with formic acid). The detection was performed by multiple reactions monitoring (MRM) mode via ESI source operating in the positive ionization mode. An linear calibration curve was obtained over the concentration range of 1.0–1000.0 ng ml−1 for lipoic acid–fasudil dimer (L–F 001). Accuracy, precision and extraction recovery of the analyte was satisfactory. The validated method was successfully applied to monitor the pharmacokinetic profile of the lipoic acid–fasudil dimer (L–F 001) after oral administration to rats.
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