Frontiers in Chemistry
·
2019
·
IF 3.782
Chen Lizhu,Yu Yingjia,Duan Gengli,Wang Xin,Shen Baohua,Xiang Ping
Objective: Chiral analysis is a crucial method to differentiate selegiline intake from drug abuse. A dried urine spot (DUS) analytical method based on spotting urine samples (10 μL) onto dried spot collection cards, and followed by air-drying and extraction, was developed and validated for the determination of selegiline, desmethylselegiline, R/S-methamphetamine, and R/S-amphetamine.Methods: Methanol (0.5 mL) was found to be the ideal extraction solvent for target extraction from DUSs under orbital-horizontal stirring on a lateral shaker at 1,450 rpm for 30 min. Determinations were performed by direct electrospray ionization tandem mass spectrometry (ESI-MS/MS) under positive electrospray ionization conditions using multiple reaction monitoring mode. The chromatographic system consisted of a ChirobioticTM V2 column (2.1 × 250 mm, 5 μm) and a mobile phase of methanol containing 0.1% (v/v) glacial acetic acid and 0.02% (v/v) ammonium hydroxide.Results and conclusions: The calibration curves were linear from 50 to 5,000 ng/mL, with r > 0.995 for all analytes, imprecisions ≤ 15% and accuracies between −11.4 and 11.7%. Extraction recoveries ranged from 48.6 to 105.4% with coefficients of variation (CV) ≤ 13.7%, and matrix effects ranged from 45.4 to 104.1% with CV ≤ 10.3%. The lower limit of quantification was 50 ng/mL for each analyte. The present method is simple, rapid (accomplished in 12 min), sensitive, and validated by a pharmacokinetic study in human urine collected after a single oral administration of SG.
研究领域:
分析化学
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药理学
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毒理学
✓ 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
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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
✓ 已验证
产品关联
DOI
PubMed
高影响因子
Chinese Herbal Medicines
·
2018
·
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
✓ 已验证
产品关联
DOI
Forensic Toxicology
·
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
✓ 已验证
产品关联
DOI
PubMed
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.
研究领域:
分析化学
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毒理学
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环境科学
✓ 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
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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
✓ 已验证
产品关联
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
✓ 已验证
产品关联
DOI
PubMed
高影响因子
Frontiers in Environmental Science
·
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
✓ 已验证
产品关联
DOI
高影响因子
Separation Science Plus
·
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
Theranostics
·
2017
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IF 8.766
Feifei Xu,Weixian Zhou,Jianxiang Cao,Qingqing Xu,Dechen Jiang,Yun Chen
The distorted and unique expression of microRNAs (miRNAs) in cancer makes them an attractive source of biomarker. There is much evidence indicating that a panel of miRNAs, termed “miRNA fingerprints”, is more specific and informative than an individual miRNA as biomarker. Thus, multiplex assays for simultaneous quantification of multiple miRNAs could be more potent in clinical practice. However, current available assays normally require pre-enrichment, amplification and labeling steps, and most of them are semi-quantitative or lack of multiplexing capability. In this study, we developed a quasi-targeted proteomics assay for multiplexed miRNA quantification by a combination of DNA-peptide probes and liquid chromatography-tandem mass spectrometry (LC-MS/MS). Specifically, the signal of target miRNAs (i.e., miR-21, miR-let7a, miR-200c, miR-125a and miR-15b) was converted into the mass response of reporter peptides by hybridization of miRNAs with DNA-peptide probes and subsequent tryptic digestion to release the peptides. After a careful optimization of conditions related to binding, conjugation, hybridization and multiple reaction monitoring (MRM) detection, the assay was validated for each miRNA and the limit of quantification (LOQ) for all the miRNAs can achieve 1 pM. Moreover, crosstalk between DNA-peptide probes in multiplex assay was sophisticatedly evaluated. Using this quasi-targeted proteomics assay, the level of target miRNAs was determined in 3 human breast cell lines and 36 matched pairs of breast tissue samples. Finally, simplex assay and qRT-PCR were also performed for a comparison. This approach grafts the strategy of targeted proteomics into miRNA quantification and may offer a new way for multiplexed miRNA profiling.
研究领域:
癌症生物学
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蛋白质组学
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分子生物学
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生物化学
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临床诊断
✓ 已验证
产品关联
DOI
PubMed
高影响因子
ANALYTICA CHIMICA ACTA
·
2024
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IF 5.7
Peiling Wu,Wenjie Wang,Chuan Huang,Le Sun,Xiaoli Wu,Lijia Xu,Peigen Xiao
Background TRY-NAD metabolic network includes TRY (tryptophan), 5-HT (5-hydroxytryptamine), KYN (kynurenine), and NAD (nicotinamide adenine dinucleotide) pathway, which plays a significant role in neurological diseases and ageing. It is important to monitor these metabolites for studying the pathological anatomy of disease and treatment of responses evaluation. Although previous studies have reported quantitative methods for several metabolites in the network, the bottlenecks of simultaneously quantifying the whole metabolic network are their similar structures, diverse physico-chemical properties, and instability. Standardized protocols for the whole metabolic network are still missing, which hinders the in-depth study of TRY-NAD metabolic network in laboratory research and clinical screening. Results We developed a LC-MS/MS method for quantifying 28 metabolites in the TRY-NAD network simultaneously. Optimization was done for the mass spectral parameters, chromatographic conditions and sample pretreatment process. The developed method was fully validated in terms of standard curves, sensitivity, carryover, recovery, matrix effect, accuracy, precision, and stability. The pretreatment of 30 samples only takes 90 minutes, and the LC-MS/MS running time of one sample is only 13 minutes. With this method, we bring to light the chaos of global TRY-NAD metabolic network in sleep deprivation mice for the first time, including serum, clotted blood cells, hippocampus, cerebral cortex, and liver. NAD pathway levels in brain and blood decreased, whereas the opposite happened in the liver. The 5-HT pathway decreased and the concentration of KYN increased significantly in the brain. The concentration of many metabolites in KYN pathway (NAD + de novo synthesis pathway) increased in the liver. Significance This method is the first time to determine the metabolites of KYN, 5-HT and NAD pathway at the same time, and it is found that TRY-NAD metabolic network will be disordered after sleep deprivation. This work clarifies the importance of the pH of the extraction solution, the time and temperature control in pretreatment in standardized protocols building, and overcoming the problems of inconsistent sample pretreatment, separation, matrix effect interference and potential metabolite degradation. This method exhibits great prospects in providing more information on metabolic disturbances caused by sleep deprivation as well as neurological diseases and ageing.
研究领域:
分析化学
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神经科学
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药理学
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生物化学
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临床研究
✓ 已验证
DOI
PubMed
高影响因子
JOURNAL OF HAZARDOUS MATERIALS
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2023
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IF 13.6
Man-Man Wang,Zi-Ling Li,Han Wu,Ke-Yan Chen,Fan Guo,Gui-Fu Zuo,Yu He,Xue-Bo Yin
Magnetic solid-phase extraction (MSPE) was developed based on a well-designed Fe 3 O 4 -NH 2 @g-C 3 N 4 nanocomposite as sorbent for a mixture of six benzophenones (BPs) in environmental water samples. The composite fabricated via in-situ self-assembled g-C 3 N 4 shell with homogeneous polymerization of cyanuric chloride and cyanuric acid on Fe 3 O 4 -NH 2 core. While high adsorption capacity was derived from g-C 3 N 4 via hydrophobic, π-π and hydrogen bonding interactions to the targets, the fast magnetic separation was realized with Fe 3 O 4 core for less solvent consumption. In combination with LC-MS/MS, the Fe 3 O 4 -NH 2 @g-C 3 N 4 sorbent minimized the interfering components, reduced the matrix effects, and provided the enrichment factors of 121–150 for six BPs with relative standard deviations ≤ 9.7% even after 20 times extraction-desorption cycles. The present method gave the detection limits of 0.3–2.5 ng/L for six BPs with the linear ranges of 1.0–2000 ng/L, and the recoveries of 84.6%−104% in sea water and 86.2%−107% in lake water samples. Thus, the Fe 3 O 4 -NH 2 @g-C 3 N 4 -based MSPE coupled with LC-MS/MS method provided a convenient, efficient, and reliable alternative to monitor trace BPs in environmental water samples.
研究领域:
环境科学
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分析化学
·
材料科学
✓ 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）