JOURNAL OF CHROMATOGRAPHY B-ANALYTICAL TECHNOLOGIES IN THE BIOMEDICAL AND LIFE SCIENCES
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2018
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IF 2.441
Qiong Lou,Jun Wen,Yuanying Jiang,Jinghua Huang,Guorong Fan,Fenyun Song
A reliable liquid chromatography/tandem mass (LC-MS/MS) method was developed for quantitation of 3′, 4′-dimethoxy flavonol-3-β- d -glucopyranoside (DF3G) in rat plasma using pantoprazole as the internal standard. An Agilent C18 column (100 mm × 3 mm, 3.5 μm) was performed for chromatographic separation with the mobile phase composed of methanol-water (containing formic acid) at a flow rate of 0.4 mL/min. A triple-quadrupole mass spectrometry equipped with an electrospray ionization (ESI) source in positive ion mode was applied to quantitative analysis by multiple reacting monitoring (MRM). The MRM precursor-product ion transition of DF3G and Pantoprazole (IS) were m / z 461.1 → 299.2 and 383.9 → 200.2, respectively. Calibration curves were recovered in a concentration range of 1–500 ng/mL for plasma with a limit of lower quantification (LLOQ) of 1 ng/mL. The intra-day and inter-day precision were not >10%. The accuracy of DF3G ranged from −10% to 0.53% in quality control (QC) samples at three concentrations. DF3G was not degraded during the analysis and the storage period. All the data were validated in accordance with the FDA bioanalytical method validation guideline. The LC-MS/MS method was successfully employed in the pharmacokinetic study of the DF3G after oral administration and intravenous injection in rats.
研究领域:
分析化学
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药物代谢
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生物医学
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产品关联
DOI
PubMed
高影响因子
Chinese Herbal Medicines
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2018
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IF 0
Xiao-jun Zhang,Jia-hui Chen,Liang Luo,Wei He,Guang-hui Liu,Jing Gong,Yi-feng Zeng,Zhi-yong Xie,Qiong-feng Liao
Objective To compare the brain pharmacokinetics of five protoberberine-type alkaloids ( i.e. berberine , palmatine , coptisine , epiberberine, and jatrorrhizine), which were the main bioactive constituents of Jiaotai Pills (JTP), in normal and insomnic rats orally administrated with JTP. Methods The detection was conducted by a fully validated liquid chromatography-tandem mass spectrometry combinated with brain microdialysis method. Brain microdialysis probes were inserted into the hippocampus of rats. JTP extracts were administrated intragastrically and then brain microdialysates were collected at 30 min time intervals for 10 h. The separation of the five protoberberine-type alkaloids was carried out on a BDS Hypersil C 18 column using a mobile phase consisting of acetonitrile and water (containing 5 mmol ammonium acetate adjusted to pH 5.0) within 4 min. The quantification was performed by multiple reaction monitoring with the transitions of m / z 336.0-320.1 for berberine, m / z 352.0-336.1 for palmatine, m / z 338.0-322.1 for jatrorrhizine , m / z 336.0-320.1 for epiberberine, m / z 320.0-292.1 for coptisine and m / z 356.4-192.1 for IS. Results The lower limit of quantification for five protoberberine-type alkaloids was 0.05 ng/mL. Linearity, accuracy, precision, stability and matrix effect of five analytes were all satisfactory. Five protoberberine-type alkaloids were quickly distributed in the brain. Moreover, significant differences in the principal pharmacokinetic parameters such as AUC and T 1/2 of the analytes were observed between two groups. Conclusion The LC-MS/MS method combinated with microdialysis is useful in the brain pharmacokinetic study of five protoberberine-type alkaloids. The results indicated that the rates of analytes absorption in insomnic rats were significantly higher than those in normal rats. Besides, the protoberberine-type alkaloids could bring a direct effect on the neuron in the hippocampus.
研究领域:
药理学
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神经科学
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分析化学
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产品关联
DOI
SCIENCE OF THE TOTAL ENVIRONMENT
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2019
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IF 5.589
Balarabe B. Ismail,Yunfeng Pu,Lihua Fan,Munir A. Dandago,Mingming Guo,Donghong Liu
Baobab ( Adansonia digitata ) fruit is a part of the baobab tree, a revered multi-purpose tree native to Africa with a myriad of potentials in providing shelter, food, medicine, clothing and as a valuable source of natural antioxidants. A massive quantity of baobab fruit shells (BFS) is generated as a waste from the baobab fruit processing representing significant economic and environmental challenges at the same time an opportunity for its valorization and commercial utilization. The present study explored the potentials of BFS as a source of phenolic compounds. For this purpose, the phenolic constituents of BFS were identified by LC-MS/QTOF analysis. Also, the Total Phenolic Chromatographic Index (TPCI), TPC, TFC, and antioxidant capacity were compared with the baobab seeds and pulp. The antidiabetic potential through α-amylase and α-glucosidase inhibitory activities was also compared with that of acarbose. The LC-MS/QTOF analysis led to the identification of 45 compounds, including quercetin, kaempferol, proanthocyanidins, phenolic acids and their derivatives, several of which had never been reported in baobab fruit. Moreover, the BFS showed higher TPC, TFC, and antioxidant capacity than the baobab seeds and pulp and inhibited α-amylase and α-glucosidase enzymes activities with much higher potency than acarbose. This research demonstrated the promising potentials of BFS as a good source of phenolic compounds that can further be utilized for food and pharmaceutical applications.
研究领域:
药用植物学
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食品科学
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分析化学
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药理学
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产品关联
DOI
PubMed
高影响因子
Forensic Toxicology
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2024
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IF 2.8
Zhang Xiaolong,Chen Yuxuan,Liu Jinlei,Wang Mengchao,Dai Yinyin,Zhao Kundi,Gu Jie,Zhang Huimin,Wurita Amin,Hasegawa Koutaro
Purpose Distribution and abuse of imidazole-derived γ-aminobutyric acid (GABA) agonists, such as etomidate and metomidate, and their analogs have been encountered frequently especially in China. The aim of this study was to identify etomidate, metomidate, propoxate, and isopropoxate more accurately by establishing a gas chromatography–mass spectrometry (GC–MS) and liquid chromatography tandem mass spectrometry (LC–MS/MS) method and applying it to real forensic cases. Methods One mg of the seized powder was dissolved in 1 mL of methanol, and subjected to GC–MS and LC–MS/MS. Hair samples were washed and cut into approximately 2 mm sections, then ground to powder by a low-temperature grinder. Twenty mg of the hair powder was extracted with 1 mL of methanol, and the supernatant was subjected to LC–MS/MS. Results Etomidate, metomidate, propoxate, and isopropoxate were chromatographically separated and each mass spectrum was obtained by GC–MS. For LC–MS/MS, tested validation data were all satisfactory. The seized powder samples contained isopropoxate, with an approximate content of 30.9%. Etomidate, etomidate acid, metomidate, and isopropoxate could be determined in the submitted hairs, ranging from 2.89 to 8.09 ng/mg, 0.0591–0.177 ng/mg, 0.342–2.77 ng/mg, and 33.2–130 ng/mg, respectively. Conclusions Mass spectra and ion chromatograms of etomidate, metomidate, isopropoxate, and propoxate were obtained by GC–MS. We have also established a simultaneous and reliable analytical method for etomidate, etomidate acid, metomidate, and isopropoxate in human hair by LC–MS/MS. This is the first report to present analytical results of a novel imidazole-derived GABA agonist isopropoxate in drug abuse cases.
研究领域:
法医学
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药物滥用检测
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分析化学
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产品关联
DOI
PubMed
高影响因子
JOURNAL OF PHARMACEUTICAL AND BIOMEDICAL ANALYSIS
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2025
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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.
研究领域:
分析化学
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毒理学
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环境科学
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产品关联
DOI
PubMed
高影响因子
JOURNAL OF CHROMATOGRAPHY B-ANALYTICAL TECHNOLOGIES IN THE BIOMEDICAL AND LIFE SCIENCES
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2014
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IF 2.694
Zhiyong Zhao,Qinxiong Rao,Suquan Song,Na Liu,Zheng Han,Jiafa Hou,Aibo Wu
A simple and reliable method for simultaneous determination of deoxynivalenol-3-glucoside and major type B trichothecenes (deoxynivalenol, nivalenol, fusarenon X, 3-acetyldeoxynivalenol, 15-acetyldeoxynivalenol and deepoxy-deoxynivalenol) in animal feed and raw materials has been developed and validated in this study. The method was based on an improved dispersive solid-phase extraction (DSPE) followed by analysis using high performance liquid chromatography coupled to tandem mass spectrometry (HPLC-MS/MS). Also, matrix-matched calibration curve ( R 2 > 0.99) was employed to minimize matrix effects and ensure accurate quantification. The recoveries during sample preparation process (including extraction and clean-up) ranged from 79.03% to 118.39%, with intra-day and inter-day relative standard deviation lower than 20% for all the analytes. The limit of quantification ranged from 5.0 μg/kg for deoxynivalenol to 13.6 μg/kg for fusarenon X. The validated method was successfully applied to the analysis of animal feed and corn. The pilot study showed that 37 out of 41 samples were contaminated with deoxynivalenol-3-glucoside at the levels of 6.0–121.0 μg/kg. Most of the type B trichothecenes were also found with the exception of fusarenon X, at the contaminated levels of 10.0–1382 μg/kg. To the best of our knowledge, this was the first scientific report on the co-occurrence of masked deoxynivalenol and type B trichothecenes in animal feed and raw materials.
研究领域:
食品安全
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分析化学
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产品关联
DOI
PubMed
高影响因子
ANALYTICAL CHEMISTRY
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2020
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IF 6.785
Shu-Jian Zheng,Jie Zheng,Cai-Feng Xiong,Hua-Ming Xiao,Shi-Jie Liu,Yu-Qi Feng
Identification of metabolites at the trace level in complex samples is still one of the major challenges in untargeted metabolomics. One formula in the metabolomic database is always corresponding to more than one candidate, which increases the difficulty and cost in the subsequent process of standard compound matching. In this study, we developed an effective method for amine metabolite identification by hydrogen–deuterium scrambling (HDS) based on chemical isotope labeling coupled with liquid chromatography–mass spectrometry (HDS–CIL–LC–MS). After d4-4-(N,N-dimethylamino)phenyl isothiocyanate (d4-DMAP) labeling, the labeled amine metabolites can produce HDS under collision-induced dissociation (CID). The HDS can effectively reflect the number of labile hydrogen atoms in amine metabolites and thus distinguish amine isomers with different functional groups. The developed HDS–CIL–LC–MS method was applied to the determination of amine metabolites in mice feces, in which the amine candidates obtained by the database based on chemical formula searching were reduced by 64% on average, which greatly reduces the cost of standard compound matching. Taken together, the developed HDS–CIL–LC–MS analysis was demonstrated to be a promising method for untargeted metabolomics and a novel strategy for deciphering tandem mass spectrometry (MS2) spectra.
研究领域:
分析化学
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代谢组学
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质谱
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产品关联
DOI
PubMed
高影响因子
ACS Omega
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2022
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IF 4.132
Prince Kumar Singh,Jagreeti Singh,Tapas Medhi,Aditya Kumar
Diabetes is a group of metabolic disorders characterized by elevated blood sugar levels, leading to many undesirable health consequences. There are many herbal formulations, traditionally used by the Northeast Indian population for disease management. These formulations require scientific validations to optimize their efficacy and increase their popularity. In this study, we attempt to scientifically validate a polyherbal formulation traditionally used for the management of diabetes through preliminary phytochemicals investigation, characterization of potential phytochemicals using Fourier transform infrared (FT-IR) spectroscopy, high-resolution liquid chromatography mass spectrometry (HR-LC/MS) analysis, and in silico characterization of physiochemical, drug-likeness, and pharmacokinetic properties of identified phytochemical compounds. Qualitative phytochemical screening of various extracts of the formulation confirmed the presence of alkaloids, phenols and tannins, flavonoids, fats, and oils. Phytochemical quantification of the various extracts showed that the highest total phenolic content is present in the ethanolic extract (35.61 ± 0.15 mg GAE/g), while the highest total flavonoid content is present in the chloroform extract (76.33 ± 2.96 mg QE/g) of the formulation. FT-IR spectroscopic analysis revealed various characteristic band values with various functional groups in the formulation extract such as amines, alcohol, fluoro compounds, phenol, alkane, alkene, and conjugated acid groups. HR-LC/MS analyses identified nearly 51 compounds including 9 small peptides and 42 potential phytochemical compounds. In silico SwissADME analysis of identified compounds revealed 25 potential compounds following Lipinski’s rule and showing drug-like characteristics, and out of them, 16 compounds exhibited good oral bioavailability, as revealed in the bioavailability radar. The overall study showed that the presented polyherbal formulation is enriched with bio-active phytochemical compounds with good pharmaceutical values.
研究领域:
药理学
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植物化学
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生物信息学
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DOI
PubMed
高影响因子
JOURNAL OF PHARMACEUTICAL AND BIOMEDICAL ANALYSIS
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2024
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IF 3.1
Fangbo Xia,Peng Cui,Ling Liu,Junhe Chen,Qiqi Zhou,Qian Wang,Hongwei Zhou
The gut microbiome plays pivotal roles in various physiological and pathological processes, with key metabolites including short chain fatty acids (SCFAs), bile acids (BAs), and tryptophan (TRP) derivatives gaining significant attention for their diverse physiological roles. However, quantifying these metabolites presents challenges due to structural similarity, low abundance, and inherent technical limitations in traditional detection methods. In this study, we developed a precise and sensitive liquid chromatography-tandem mass spectrometry (LC-MS/MS) method utilizing a chemical isotope derivatization technique employing 4-(aminomethyl)-N,N-dimethylaniline- d 0 / d 6 (4-AND- d 0 / d 6 ) reagents to quantify 37 typical gut microbiome-derived metabolites. This method achieved an impressive 1500-fold enhancement in sensitivity for detecting metabolites, compared to methods using non-derivatized, intact molecules. Moreover, the quantitative accuracy of our chemical isotope derivatization strategy proved comparable to the stable isotope labeled internal standards (SIL-IS) method. Subsequently, we successfully applied this newly developed method to quantify target metabolites in plasma, brain, and fecal samples obtained from a neonatal hypoxic-ischemic encephalopathy (HIE) rat model. The aim was to identify crucial metabolites associated with the progression of HIE. Overall, our sensitive and reliable quantification method holds promise in elucidating the role of gut microbiome metabolites in the pathogenesis of various diseases.
研究领域:
医学
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代谢组学
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神经科学
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产品关联
DOI
PubMed
高影响因子
Frontiers in Environmental Science
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2021
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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.
研究领域:
环境科学
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分析化学
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药物分析
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产品关联
DOI
高影响因子
JOURNAL OF CHROMATOGRAPHY A
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2025
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IF 4
Xijia Zhang,Yingjie Zhuo,Qianqian Xu,Ningning Wang,Hao Zhong,Dongsheng Li,Juanjuan Zhao
Steroid hormones play a crucial role in human physiological functions, and the simultaneous quantification of multiple steroid hormones in biological matrices has considerable clinical relevance. However, the simultaneous quantification of steroid hormones in biological matrices remains analytically challenging due to their ultra-trace concentrations and substantial matrix interference. A novel complementary multi-aptamer strategy was proposed in our study. Multi-aptamer magnetic beads (MA-MBs) were synthesized by simultaneously immobilizing estrogen-specific aptamer (AptE) and corticoid-specific aptamer (AptC) on the magnetic beads. Then MA-MBs was used to extract multiple steroid hormones in biological matrices based on the combined specificity of complementary aptamers. Following extraction, the enriched steroid hormones are quantified using quadrupole time-of-flight liquid chromatography-mass spectrometry (Q-TOF LC-MS). MA-MBs demonstrated a rapid magnetic response (5 seconds), high extraction efficiency, and excellent reusability (at least 10 cycles). Under optimal extraction conditions, the proposed MA-MBs-Q-TOF LC-MS method exhibited a wide linear range (0.02-200 ng/mL), low limits of detection (0.02-1 ng/mL), and high recovery rates (92.93%-104.93%) for 10 types of steroid hormones. Finally, the validated method was applied to quantify ten clinically-relevant steroid hormones in serum samples, demonstrating its potential for advanced endocrine research applications. Furthermore, this study provides a robust platform for multiplexed targets analysis in complex biological matrices.
研究领域:
分析化学
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内分泌学
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生物分析化学
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质谱分析
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分子识别
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产品关联
DOI
PubMed
高影响因子
Separation Science Plus
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2025
·Vol. 8
·期 8
·e70105
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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.
研究领域:
中医药
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药理学
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分析化学
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呼吸系统疾病
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工艺优化
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质谱分析
✓ 已验证
产品关联
DOI
高影响因子
危险品化学品经营许可证（带存储）