JOURNAL OF SEPARATION SCIENCE
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2016
·Vol. 40
·期 3
·725-732
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IF 2.741
Jing Sun,Xian-En Zhao,Jun Dang,Xiaoyan Sun,Longfang Zheng,Jinmao You,Xiao Wang
In this work, a hyphenated technique of dual ultrasound-assisted dispersive liquid–liquid microextraction combined with microwave-assisted derivatization followed by ultra high performance liquid chromatography tandem mass spectrometry has been developed for the determination of phytosterols in functional foods and medicinal herbs. Multiple reaction monitoring mode was used for the tandem mass spectrometry detection. A mass spectrometry sensitive reagent, 4′-carboxy-substituted rosamine, has been used as the derivatization reagent for five phytosterols, and internal standard diosgenin was used for the first time. Parameters for the dual microextraction, microwave-assisted derivatization, and ultra high performance liquid chromatography tandem mass spectrometry were all optimized in detail. Satisfactory linearity, recovery, repeatability, accuracy and precision, absence of matrix effect, extremely low limits of detection (0.005–0.015 ng/mL) and limits of quantification (0.030–0.10 ng/mL) were achieved. The proposed method was compared with previously reported methods. It showed better sensitivity, selectivity, and accuracy. The matrix effect was also significantly reduced. The proposed method was successfully applied to the determination of five phytosterols in vegetable oil (sunflower oil, olive oil, corn oil, peanut oil), milk and orange juice (soymilk, peanut milk, orange juice), and medicinal herbs (Ginseng, Ganoderma lucidum, Cordyceps, Polygonum multiflorum) for the quality control of functional foods and medicinal herbs.
研究领域:
分析化学
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食品科学
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中药学
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DOI
高影响因子
MICROCHEMICAL JOURNAL
·
2025
·
IF 5.1
Yun Wu,Yanqun Yang,Ming Wen,Jing Xie,Linchun Bao,Shuting Yang,Xiangming Luo,Xingyi Wang,Qianchun Zhang
Monoamine neurotransmitters play vital roles in cognitive and various physiological and pathophysiological processes, but their trace levels, small sample volumes, and complex biological matrices in biological samples pose significant analytical challenges. This study developed a novel method for the simultaneous quantification of six monoamine neurotransmitters—tyrosine, vanillylmandelic acid, tryptophan, 3,4-dihydroxyphenylacetic acid, 5-hydroxyindole-3-acetic acid, and homovanillic acid—in human serum and urine. The method utilizes magnetic solid-phase extraction coupled with ultra-high-performance liquid chromatography-tandem mass spectrometry (UHPLC-MS/MS). A multifunctional magnetic composite, polyethylenimine@polymer dopamine hydrochloride@NH 2 -MIL-53(Al)-SiO 2 @Fe 3 O 4 , was synthesized, exhibiting high extraction selectivity and capacity and achieving an extraction range of 9.61–25.4 nmol/mg for the target neurotransmitters. The analytical method, optimized for the aforementioned composite, exhibited robust linearity for all six monoamine neurotransmitters, with correlation coefficients ( R 2 ) exceeding 0.998. The limits of detection (S/N = 3) ranged from 1.1 to 22 ng/L, indicating high sensitivity. Recovery rates for the targeted analytes varied between 94.5 % and 112 %, and relative standard deviations remained within the range of 1.5–9.4 %. These findings confirm that the developed methodology is sensitive, accurate, selective, and reliable for the quantitative determination of trace monoamine neurotransmitters in complex biological samples.
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DOI
高影响因子
JOURNAL OF CHROMATOGRAPHIC SCIENCE
·
2023
·
IF 1.3
Xia Chenjie,Zhu Hongliu,Hu Changhui,Liu Jie,Hua Haibing,Yang Jianqiu,Chen Zhipeng,Gao Yihong
Pinus massoniana needles, a traditional herb, were applied to prevent hair loss in China. Studies available mainly focused on pine needle flavonoids with various biological activities. However, there has been no pharmacokinetics study of the flavonoids from Pinus needles extract. A selective and sensitive ultra-high performance liquid chromatography–tandem mass spectrometry (UHPLC-MS/MS) method was developed to simultaneously quantify taxifolin, quercetin and catechin in rat plasma. To separate the three constituents, an Agilent Extend-C18 column (2.1 mm × 100 mm, 1.8 μm) was used with a mobile phrase of (A) 0.1% formic acid and (B) acetonitrile. The analytes were measured by multiple reaction monitoring in the negative ionization mode. There was good linearity in the established UHPLC-MS/MS method, with a coefficient of determination (r2) of >0.99. The accuracy, intra-day and inter-day precision and recovery were all satisfactory and these 3 compounds were stable under the tested conditions. The validated method in this study was successfully applied to pharmacokinetic study in healthy rats after oral and transdermal administration of Pinus needles extract. The results could provide further research foundation for pine needle extract as external preparations.
研究领域:
中药学
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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
JOURNAL OF CHROMATOGRAPHY B-ANALYTICAL TECHNOLOGIES IN THE BIOMEDICAL AND LIFE SCIENCES
·
2024
·
IF 2.8
Xiaoxue Xu,Sheng Guo,Jiangyan Chen,Yuhan Song,Xueli Wu,Feng Liu,Jin-Ao Duan
The Zingiberis Rhizoma − Jujubae Fructus herb pair (ZJHP) is a classic herb pair in traditional Chinese medicine. The herb pair shows the effect of dispelling cold, harmonizing the middle and improving gastrointestinal function, and is widely used for patients with stomach cold syndrome (SCS), stomachache and anemofrigid cold. The gingerols, shogaols, flavonoids and triterpenic acids are the important bioactive ingredients of ZJHP. However, few pharmacokinetic studies have been investigated in vivo for the above compounds. To comprehend the kinetics of active components and promote their curative application, a fast and sensitive ultra-high performance liquid chromatography coupled with mass spectrometry (UHPLC-MS/MS) method was established for simultaneous determination of 12 analytes in normal and SCS rats in this study. The results showed that the pharmacokinetic parameters (C max , T max , t 1/2z , MRT 0-t , AUC 0-t and AUC 0-∞ ) in SCS model were significantly different from those in normal rats. In addition, the pharmacokinetics of rats given ZJHP were also varied from single herb oral administration, especially in model condition. These results indicated that the in vivo processes of the above analytes changed under pathological conditions and the compatibility of the herb pair could significantly influence the absorption of active components, which might provide an insight and further supports for the clinical application of ZJHP.
研究领域:
药理学
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中药学
·
分析化学
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DOI
PubMed
高影响因子
ANALYTICAL LETTERS
·
2021
·
IF 2.329
Qian Wang,Li Zhu,Yi Yu,Huashi Guan,Zhe Xu
Aminoglycoside antibiotics exhibit broad-spectrum antibacterial activity, good efficacy, and stability. However, due to the emergence of antibiotic resistance, their use as broad-spectrum antibiotics is restricted. Bacteria producing the bifunctional enzyme, 6′-aminoglycoside acetyltransferase 2″-aminoglycoside phosphotransferase [AAC(6′)-APH(2″)], can modify aminoglycoside antibiotics, leading to the emergence of clinical drug resistance. A method based on ultra-high performance liquid chromatography–mass spectrometry (UHPLC-MS) is reported to monitor the modification of aminoglycoside antibiotics and to screen potential inhibitors of AAC(6′)-APH(2″) from marine natural products. Instead of using purified AAC(6′)-APH(2″), Escherichia coli cells harboring AAC(6′)-APH(2″) were employed. In vivo enzyme assays, conducted in the physiological environment, compensated for the disparity between in vitro responses and those in living cells. The inhibition zone method was used to verify the reliability of the UHPLC-MS results. From a library of 63 marine natural products, Mer-C-3 and Mer-c-8e pyridine alkaloids were shown to provide inhibitory activity against AAC(6′)-APH(2″) in living bacteria. The UHPLC-MS-based approach offers improved speed, convenience, and sensitivity compared with the traditional inhibition zone assay for the screening of enzyme inhibitors.
研究领域:
微生物学
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分析化学
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药理学
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DOI
高影响因子
Analytical Methods
·
2016
·Vol. 9
·期 3
·482-489
·
IF 1.915
Hua Dang,Donghong Liu,Xiangchang Hou,Yuluan Wu,Bin Wang,Hao Dong,Yanping Xian
One-step extraction prior to a two-step detection method based on UHPLC-MS/MS was developed to determine seven quaternary ammonium salts (QACs), three isothiazolinone antibacterial agents and seven phenolic antibacterial agents in infant disposable hygiene products. Samples were ultrasonically extracted by acetonitrile; the extraction solution was directly used to separate seven QACs on a hydrophilic chromatographic column (HILIC column) by isocratic elution (0.1% formic acid acetonitrile and 10 mmol L−1 ammonium acetate solution as the mobile phases). QACs were then detected in multiple reaction monitoring (MRM) of MS/MS under an electro-spray ionization source in positive mode (ESI+). For the remaining ten analytes, the extraction solution was dried by nitrogen gas blowing and re-dissolved with acidulated methanol water solution. Then they were separated on a C18 chromatographic column with gradient elution program using methanol and water as mobile phases. Finally, ten analytes were simultaneously ionized by using a electro-spray source in positive and negative modes and acquisition was achieved in MRM. The developed methods were validated in terms of the method limit of detection and quantitation (MLOD and MLOQ), matrix effects, recovery and precision. Results indicated that favorable linear relations (r > 0.997) were obtained over the selected concentration ranges of 0.1–50 μg L−1, 1.0–500 μg L−1 and 50–2000 μg L−1 for QACs, isothiazolinone antibacterial agents and phenolic antibacterial agents, respectively. The MLODs of the three groups of antibacterial agents were 0.8 μg kg−1, 1.5–6.5 μg kg−1 and 200–500 μg kg−1, respectively. Recoveries were calculated at three concentration levels spiked in negative paper diaper samples and the values were found between 83.7% and 112% with relative standard deviation (RSD) values less than 13% for intra-day precision (n = 6) and less than 16% for inter-day precision (n = 5). The developed and validated methods were successfully applied to determine the concentrations of antibacterial agents in real samples and QACs and isothiazolinone antibacterial agents were detected in several samples. These methods are rapid, sensitive and suitable for the determination of antibacterial agents in infant disposable hygiene products and some other similar products.
研究领域:
分析化学
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环境科学
·
公共卫生
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产品关联
DOI
高影响因子
NEW JOURNAL OF CHEMISTRY
·
2018
·Vol. 42
·期 24
·19578-19590
·
IF 3.201
Xucan Yuan,Di Wu,Chu Liu,Xianhui Li,Zhili Xiong,Longshan Zhao
A sensitive and accurate analytical method, magnetic solid-phase extraction combined with dispersive liquid–liquid microextraction followed by ultra-high performance liquid chromatography-tandem mass spectrometry, was established for the simultaneous quantification of eight sulfonamide antibiotics in environmental water samples. In this study, a magnetic nanocomposite, polypyrrole-modified magnetic multi-walled carbon nanotubes, was prepared, characterized and applied as an efficient adsorbent for magnetic solid-phase extraction. The synthetic material exhibited satisfactory adsorption capacity for sulfonamides. Moreover, the sample pretreatment-combined technology of magnetic solid-phase extraction and dispersive liquid–liquid microextraction exhibited better purification ability than only magnetic solid-phase extraction. Furthermore, the various extraction parameters affecting the extraction efficiency were thoroughly optimized. Under the optimized conditions, high sensitivity was achieved with method detection limits in the range of 1.02–2.97 ng L−1 and method quantitation limits in the range of 3.05–9.89 ng L−1. The recovery of eight sulfonamides in five environmental water samples was in the range of 78.3–95.6% and the relative standard deviations were no more than 8.5%. Finally, the method was successfully applied to the analysis of sulfonamides in real environmental water samples (river water, lake water, influent wastewater, effluent wastewater and farm wastewater). Accordingly, the newly established method is reliable for monitoring sulfonamide residues in complex environmental matrices, which has great significance for evaluating the effects of sulfonamide residues on humans and the ecosystem.
研究领域:
分析化学
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环境科学
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产品关联
DOI
高影响因子
Journal of Chemistry
·
2021
·
IF 2.506
Yuqing Wang,Jianming Wu,Yunxia Li,Jing Yang,Long Wang,Anguo Wu,Feihong Huang,Nan Jiang,Can Tang,Yan Li
To investigate the pharmacokinetics of 2, 3, 8-trimethylellagic (TMEA) in rats in vivo and determine the possible effects of the pathological conditions and compatibility, a rapid and sensitive ultra-high-performance liquid chromatography-tandem mass spectrometry (UHPLC-MS/MS) method for quantitative determination was developed. TMEA and Artemetin (internal standard, IS) were separated on an Acquity Shim-pack GIST column with a total running time of 7 min using gradient elution at a flow rate of 0.3 mL/min. The intraday and interday relative standard deviations were <9.50%, and the relative error of accuracy was between −5.70% and 2.96%. The calibration curve of TMEA demonstrated good linearity with r2 = 0.9996, with the average recovery changing from 94.77% to 102.47% and the matrix effect from 93.16% to 100.15%. Compared with the normal group, the area under the plasma concentration-time curve from time 0 to the last time of quantifiable concentration (AUC(0 − t)), area under the plasma concentration-time curve from time 0 extrapolated to infinite time (AUC(0 − ∞)), and the maximum concentration (Cmax) of TMEA increased, whereas the time of maximum concentration (Tmax) and apparent clearance (CL/F) remarkably decreased in the TMEA group. With significantly reduced CL/F, AUC(0 − t), AUC(0 − ∞), and Cmax for TMEA were increased approximately one time after combining with 3, 7-Di-O-methylducheside A (DOMA). AUC(0 − t) and Cmax for TMEA in the 2, 3, 8-trimethylellagic-3, 8-dimethoxyellagic acid-2-oxyglucoside (TMEA-DMAG) group were significantly lower than that in the TMEA group with clearly prolonged Tmax and increased CL/F. These findings indicate that the changes in the pharmacokinetic parameters of TMEA may be caused by pathological and combination conditions.
研究领域:
药理学
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分析化学
·
中药学
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产品关联
DOI
高影响因子
ANALYTICAL LETTERS
·
2021
·
IF 2.329
Zhao Jin,Guanyu Zou,Xintao Mao,Shanshan Guan,Wenna Guan
A rapid and sensitive method was developed determine free fatty acids in cyanobacteria extracellular medium without derivatization by stir bar sorptive extraction (SBSE) coupled to ultra-high-performance liquid chromatography – tandem mass spectrometry (UHPLC-MS/MS). The stir bars (20 mm in length and 1 mm in film thickness) coated with polydimethylsiloxane was used to directly extract 11 free fatty acids (C14-C24) in cyanobacteria extracellular media. The performance was optimized, including the column, temperature, extraction time, organic modifier, and desorption solvent. Limits of detection and quantification, precision, and linear dynamic ranges for the free fatty acids were evaluated. The method was applied to determine free fatty acids in cyanobacteria extracellular media at the exponential and plateau phases. Eicosanoic acid (C20:0), linoleic acid (C18:2), oleic acid (C18:1), stearic acid (C18:0), palmitic acid (C16:0) and myristic acid (C14:0) were quantified in the samples.
研究领域:
分析化学
·
环境科学
·
生物技术
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产品关联
DOI
高影响因子
MOLECULES
·
2019
·Vol. 24
·期 7
·1440
·
IF 3.06
Huang-qin Zhang,Pei Liu,Jin-ao Duan,Ling Dong,Er-xin Shang,Da-wei Qian,Zhen-hua Zhu,Hui-wei Li,Wei-wen Li
Trichosanthes kirilowiiMaxim. is one of the original plants for traditional Chinese medicines Trichosanthis Fructus, Trichosanthis Semen, Trichosanthis Pericarpium and Trichosanthis Radix. Amino acids, nucleosides and carbohydrates are usually considered to have nutritional value and health-care efficacy. In this study, methods involving high-performance liquid chromatography coupled with evaporative light scattering detector (HPLC-ELSD), UV-visible spectrophotometry and ultra-high-performance liquid chromatography coupled with tandem mass spectrometry (UHPLC-MS/MS) were established for quantifying carbohydrates (fructose, glucose, stachyose, raffinose and polysaccharide), fourteen nucleosides and twenty one amino acids. Moreover, sixty-three samples from nine different parts, including pericarp, seed, fruit pulp, stem, leaf, main root, main root bark, lateral root and lateral root bark ofT. kirilowiifrom different cultivated varieties were examined. The established methods were validated with good linearity, precision, repeatability, stability, and recovery. The results showed that the average content of total amino acids in roots (15.39 mg/g) and root barks (16.38 mg/g) were relatively higher than for others. Contents of nucleosides in all parts ofT. kirilowiiwere below 1.5 mg/g. For carbohydrates, fruit pulp has a higher content than others for glucose (22.91%), fructose (20.63%) and polysaccharides (27.29%). By using partial least-squared discriminate analysis (PLS-DA), Variable importance in the projection (VIP) plots and analysis of variance (ANOVA) analysis, the characteristic components of the different organs (fruit, stems and leaves, roots) were found. This analysis suggested there were potential medicinal and nutritive health care values in various parts of theT. kirilowii, which provided valuable information for the development and utilization ofT. kirilowii.Keywords:Trichosanthes kirilowiiMaxim;different parts;carbohydrate;nucleosides;amino acids;resource utilization
研究领域:
生药学
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分析化学
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中药学
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产品关联
DOI
PubMed
高影响因子
MICROCHIMICA ACTA
·
2024
·Vol. 191
·期 6
·1-11
·
IF 5.3
Zhou Wenxiu,Lv Xiaoyuan,Zhang Shengman,Gao Zhenye,Li Bingjie,Wang Xin
A novel in-tube solid-phase microextraction coupled with an ultra-high performance liquid chromatography-mass spectrometry method has been established for simultaneous quantification of three crucial brain biomarkers N -acetylaspartic acid (NAA), N -acetylglutamic acid (NAG), and N -acetylaspartylglutamic acid (NAAG). A polymer monolith with quaternary ammonium as the functional group was designed and exhibited efficient enrichment of target analytes through strong anion exchange interaction. Under the optimized conditions, the proposed method displayed wide linear ranges (0.1–80 nM for NAA and NAG, 0.2–160 nM for NAAG) with good precision (RSDs were lower than 15%) and low limits of detection (0.019–0.052 nM), which is by far the most sensitive approach for NAA, NAG, and NAAG determination. Furthermore, this approach has been applied to measure the target analytes in mouse brain samples, and endogenous NAA, NAG, and NAAG were successfully detected and quantified from only around 5 mg of cerebral cortex, cerebellum, and hippocampus. Compared with existing methods, the newly developed method in the current study provides highest sensitivity and lowest sample consumption for NAA, NAG, and NAAG measurements, which would potentially be utilized in determining and tracking these meaningful brain biomarkers in diseases or treatment processes, benefiting the investigations of pathophysiology and treatment of brain disorders. Graphical abstract
研究领域:
分析化学
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神经化学
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生物医学
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产品关联
DOI
PubMed
高影响因子
ACS Chemical Neuroscience
·
2021
·
IF 4.418
Peng Wang,Xiaoxia Gao,Fang Zhao,Yao Gao,Kexin Wang,Jun-Sheng Tian,Zhenyu Li,Xue-Mei Qin
Depression has drawn increasing attention from the public around the world in recent years. Studies have shown that liver injury caused by chronic stress is relevant to depression and neurotransmitter changes. It is essential to clarify the relationship between neurotransmitter changes and hepatic gene expression in depression. In this study, we used the chronic unpredictable mild stress (CUMS) model combined with UHPLC–MS to explore the changes of neurotransmitters in serum and hippocampus and to decipher the differential gene expression in the liver by using the RNA-Seq combined with multivariate statistical analysis. Compared with the control group, the levels of neurotransmitters including 5-hydroxytryptamine (5-HT), acetylcholine, glutamate (Glu), and dopamine (DA) in the hippocampus and 5-HT, norepinephrine, γ-aminobutyric acid (GABA), and 5-hydroxyindoleacetic acid in serum were significantly changed in the CUMS rats. The results of liver transcriptomic analysis and correlation analysis showed that the Glu, DA, 5-HT, and GABA were impacted by 68 liver genes which were mainly enriched in three pathways including circadian rhythm, serotonergic synapse, and p53 signaling pathway. The expressive levels of clock genes and serotonergic synapse genes were validated by using q-PCR, and the diurnal rhythms of neurotransmitters were validated by in vivo hippocampus microdialysis. The CUMS stressors might cause phase advance of Glu and GABA by adjusting clock genes. The transcriptomic technique combined with correlation analysis and in vivo microdialysis could be used to discover comprehensive pathways of depression. It provides a new strategy for the rational assessment of the mechanism of disease.
研究领域:
神经科学
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药理学
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分子生物学
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转录组学
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行为科学
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DOI
PubMed
高影响因子
危险品化学品经营许可证（带存储）