JOURNAL OF PHARMACEUTICAL AND BIOMEDICAL ANALYSIS
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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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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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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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Chemistry Central Journal
·
2014
·Vol. 8
·期 1
·1-10
·
IF 1.663
Chen Feng,Li Hai-Long,Tan Yin-Feng,Guan Wei-Wei,Li Yong-Hui,Zhang Jun-Qing
Background Yakuchinone A has a plethora of beneficial biological effects. However, the pharmacokinetic (PK) data of yakuchinone A still remain unknown so far. Furthermore, the quantification of yakuchinone A in biological samples has not been reported in the literature. Therefore, in the present study we aimed to develop a new method for the fast, efficient and accurate assessment of yakuchinone A concentration in plasma, as a means for facilitating the PK evaluation of yakuchinone A.Results A liquid chromatography-electrospray ionization-tandem mass spectrometry (LC-ESI-MS/MS) method was developed and validated for the determination of yakuchinone A in rat plasma. Mass spectrometric and chromatographic conditions were optimized. Plasma samples were pretreated by protein precipitation with methanol. LC separation was performed on a Phenomenex Luna C18 column with gradient elution using a mobile phase consisting of methanol–water containing 0.5 mM formic acid (HCOOH) at a flow rate of 0.28 mL/min. ESI-MS spectra were acquired in positive ion multiple reaction monitoring mode (MRM). The precursor-to-product ion pairs used for MRM of yakuchinone A and yakuchinone B were m/z 313.1 → 137.0 and 311.2 → 117.1, respectively. Low concentration of HCOOH reduced the ion suppression caused by matrix components and clearly improved the analytical sensitivity. Yakuchinone A showed good linearity over a wide concentration range (r > 0.99). The accuracy, precision, stability and linearity were found to be within the acceptable criteria. This new method was successfully applied to analyze the rat plasma concentration of parent yakuchinone A after a single oral administration of SuoQuan capsules. Low systemic exposure to parent yakuchinone A was observed.Conclusion The proposed method is sensitive and reliable. It is hoped that this new method will prove useful for the future PK studies.
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Analytical Methods
·
2014
·Vol. 6
·期 21
·8675-8681
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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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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.
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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 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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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.
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LWT-FOOD SCIENCE AND TECHNOLOGY
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2025
·
IF 6.6
Mingzheng Duan,Ting Jiang,Xi Wang,Kangjian Song,Xu Xiao,Xiaoting Fu,Sijiu He,Jieming Feng,Muhammad Junaid Rao,Hengcui Guo
Strawberries ( Fragaria × ananassa ) are prized for bioactive flavonoids and anthocyanins, contributing to antioxidant capacity and health benefits. However, decades of breeding for yield and shelf-life have eroded their phytochemical diversity. To explore this trade-off, we compared wild strawberries ( Fragaria nilgerrensis , HM) with three cultivated varieties (pink-FY, red-RF, white-DX) using integrated LC-MS/MS metabolomics and transcriptomics. Wild HM strawberries contained twice the vitamin C (134.2 mg/100g), 2.5× more total flavonoids (138.7 mg/100g), and higher antioxidant activity (367 μg Trolox/g) than commercial varieties. In contrast, red-fruited RF showed abundant anthocyanins (pelargonidin-3-glucoside 6.6% abundance), while the wild HM genotype accumulated higher levels of flavonoids, with neohesperidin, lonicerin, hyperin and ternatumoside II collectively representing 20.9% of total flavonoids - concentrations 3-169 times greater than those observed in the three commercial varieties (FY, RF, DX). Transcriptomic analysis (RNA-seq, Illumina HiSeq 2500) revealed distinct MYB transcription factor associations: FxaYL_611g0111200 (MYB66) showed strong positive correlation with anthocyanin biosynthesis in RF (r=0.92, **p<0.005 ), while FxaYL_242g0472670 (MYB44-like) was significantly associated with HM's unique antioxidant flavonoid profile (r=0.96, ***p<0.0001 ). These regulatory relationships were corroborated by hierarchical clustering demonstrating varietal-specific expression patterns and principal component analysis (82.6% variance explained), collectively providing molecular targets for enhancing nutritional quality in strawberry breeding programs.
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Separation Science Plus
·
2025
·Vol. 8
·期 8
·e70105
·
IF 1.6
Wenya Xu,Hailing Wang,Yan Sun,Haojie Li,Jue Song
The fatty oil in Sanzi Yangqin Decoction is a crucial medicinal ingredient found in this renowned traditional Chinese medicine formula for the treatment of chronic obstructive pulmonary disease (COPD). However, a disadvantage of the extraction process using the conventional decoction approach is the poor extraction rate. In this study, we employed network pharmacology to screen for active components for the treatment of COPD, and we optimized the extraction procedure of the fatty oil of Sanzi Yangqin Decoction with the Box–Behnken response surface test. Based on the single-factor experiment and the Box–Behnken response surface test, the liquid chromatography-triple quadrupole mass spectrometry method (LC-MS/MS) to measure these four components has been constructed with the extraction time, extraction temperature, and liquid-to-feed ratio as examining factors and the composite scores of the extracted amounts of the four components as examining indexes. According to the results of the study, luteolin, arachidonic acid, sinoacutine, and sinapine thiocyanate have been selected as the analytes for determining the fat oil content of Sanzi Yangqin Decoction. The most effective extraction conditions were 4.1 h, 92°C, and a liquid-to-feed ratio of 10:1 mL/g, which achieved a composite score of 85.1. The methodological analysis of the LC-MS/MS methodology demonstrated that the precision, repeatability, and sample recovery all proved effective, and the linear relationship was good within the range of the four constituents. The optimized Sanzi Yangqin Decoction fatty oil extraction process is reasonable and feasible. And the LC-MS/MS content determination method is simple, rapid, sensitive, and specific. This work introduces an innovative approach to examining the fatty oils in Sanzi Yangqin Decoction.
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JOURNAL OF PHARMACEUTICAL AND BIOMEDICAL ANALYSIS
·
2017
·
IF 3.255
Katerina Grigori,Yannis L. Loukas,Anđelija Malenović,Vicky Samara,Anastasia Kalaskani,Efi Dimovasili,Magda Kalovidouri,Yannis Dotsikas
A sensitive Liquid Chromatography tandem mass spectrometry (LC–MS/MS) method was developed and validated for the quantitative analysis of three potential genotoxic impurities (318BP, M9, S5) in meropenem Active Pharmaceutical Ingredient (API). Due to the requirement for LOD values in ppb range, a high concentration of meropenem API (30 mg/mL) had to be injected. Therefore, efficient determination of meropenem from its impurities became a critical aim of this study, in order to divert meropenem to waste, via a switching valve. After the selection of the important factors affecting analytes’ elution, a Box-Behnken design was utilized to set the plan of experiments conducted with UV detector. As responses, the separation factor s between the last eluting impurity and meropenem, as well as meropenem retention factor k were used. Grid point search methodology was implemented aiming to obtain the optimal conditions that simultaneously comply to the conflicted criteria. Optimal mobile phase consisted of ACN, methanol and 0.09% HCOOH at a ratio 71/3.5/15.5 v/v. All impurities and internal standard omeprazole were eluted before 7.5 min and at 8.0 min the eluents were directed to waste. The protocol was transferred to LC–MS/MS and validated according to ICH guidelines.
研究领域:
分析化学
·
药物分析
·
药学
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