JOURNAL OF SEPARATION SCIENCE
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2019
·Vol. 43
·期 3
·590-597
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IF 2.516
Hong Pan,Feng Yang,Daiyuan Xiang,Fuguo Shi
Xanthii Fructus is extensively used as an herbal medicine. Ingestion of this herb is associated with severe hepatotoxicity and nephrotoxicity. Atractyloside and carboxyatractyloside are two dominative toxic constituents in Xanthii Fructus. However, their pharmacokinetic study is lacking. In this study, a novel high-performance liquid chromatography-tandem mass spectrometry method was developed to simultaneously quantify the rat plasma concentrations of atractyloside and carboxyatractyloside. After protein precipitation, the analytes were chromatographic separated on a ZORBAX Eclipse Plus column (2.1 × 150 mm id, 5 µm) under gradient elute. In the negative electrospray ionization mode, the transitions at m/z 725.3→645.4 for atractyloside, m/z 769.3→689.4 for carboxyatractyloside, and m/z 479.2→121.1 for paeoniflorin (the internal standard) were acquired by multiple reaction monitoring. This analytical method showed good linearity over 1–500 ng/mL for atractyloside and 2–500 ng/mL for carboxyatractyloside with acceptable precision and accuracy. No matrix effect, instability and carryover occurred in the analysis procedure. The extraction recoveries were greater than 85.0%. This method was applied to a preliminary pharmacokinetic study by orally administering Xanthii Fructus extract (9 g/kg) to rats, which was useful to evaluate the role of these two compounds in Xanthii Fructus-induced toxicity.
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BIOMEDICAL CHROMATOGRAPHY
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2015
·Vol. 29
·期 11
·1737-1743
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IF 1.723
Xue-jia Zhai,Fen Chen,Chao-ran Zhu,Yong-ning Lu
Many amino acid neurotransmitters in urine are associated with chronic stress as well as major depressive disorders. To better understand depression, an analytical LC-MS/MS method for the simultaneous determination of 11 underivatized neurotransmitters (4-aminohippurate, 5-HIAA, glutamate, glutamine, hippurate, pimelate, proline, tryptophan, tyramine, tyrosine and valine) in a single analytical run was developed. The advantage of this method is the simple preparation in that there is no need to deconjugate the urine samples. The quantification range was 25–12,800 ng mL −1 with >85.8% recovery for all analytes. The nocturnal urine concentrations of the 11 neurotransmitters in chronic unpredictable mild stress (CUMS) model rats and control group ( n = 12) were analyzed. A series of significant changes in urinary excretion of neurotransmitters could be detected: the urinary glutamate, glutamine, hippurate and tyramine concentrations were significantly lower in the CUMS group. In addition, the urinary concentrations of tryptophan as well as tyrosine were significantly higher in chronically stressed rats. This method allows the assessment of the neurotransmitters associated with CUMS in rat urine in a single analytical run, making it suitable for implementation as a routine technique in depression research. Copyright © 2015 John Wiley & Sons, Ltd.
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JOURNAL OF CHROMATOGRAPHY B-ANALYTICAL TECHNOLOGIES IN THE BIOMEDICAL AND LIFE SCIENCES
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2014
·
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.
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JOURNAL OF AGRICULTURAL AND FOOD CHEMISTRY
·
2015
·
IF 2.912
Xin Li,Man-Man Wang,Guo-Ying Zheng,Lian-Feng Ai,Xue-Sheng Wang
A hydrophobic monolith (10 mm × 2.1 mm i.d.) was developed as a reusable online solid-phase extraction (SPE) sorbent coupled with LC-MS/MS for the rapid determination of five avermectin residues in foodstuffs of both plant and animal origin. The online SPE was achieved using a 10 mmol/L ammonium acetate solution as the loading solvent, and acetonitrile (MeCN) was selected for the washing step. After being transferred from the monolith into a C18 analytical column using MeCN, the analytes were analyzed by LC-MS/MS using MeCN/0.1% NH4OH (10:90, v/v) as the mobile phase. The detection limit was 2 μg/kg for five avermectins, and the recoveries in fresh pear, chili seed, bovine muscle, and milk ranged from 71.8% to 101.3% with relative standard deviations of less than 8.94%. The online SPE and determination were achieved within 15 min, and the monolithic extractor was reusable for more than 500 experiments.
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JOURNAL OF NUTRITIONAL BIOCHEMISTRY
·
2024
·
IF 4.8
Yiming Ni,Xinghua Chen,Yiqun Jia,Long Chen,Mingmei Zhou
Currently, the hepatoprotective activity of taxifolin, a flavonoid isolated from Pseudotsuga taxifolia , has been reported in many animal models. However, whether the protective effect of taxifolin on the liver is related to its effect on lipidomics is unclear. Based on the significant therapeutic effect of taxifolin on CCl 4 induced subacute hepatic injury, we observed the intervention of taxifolin by lipidomics. The results demonstrate that taxifolin can effectively reverse the damage caused by CCl 4 , which including hepatocyte vacuolization and necrosis. Lipomic profiling based on liquid chromatography-mass spectrometry showed that taxifolin was able to restore lipidomic changes caused by CCl 4 , including the levels of lysophosphatidylserine (LPS), phosphatidylcholine (PC), coenzyme (Co), phosphatidylglyceride (PG), phosphatidylserine (PS), dimethylphosphatidylethanolamine (dMePE), ceramide (Cer), sphingosine (So), triglycerides (TG), and monogalactosyl diacylglycerol (MGDG) in the rat liver, and phosphatidylcarbinol (PMe) and phosphatidylethanolamine (PE), plant sphingosine (phSM), glucose ceramide (CerG1), TG, and diglycerides (DG) in serum. Spearman's correlation analysis showed that CerG1, phSM, PE, and PMe in serum, and Cer, dMePE, PG, PS, So, TG, and MGDG in liver were positively correlated with serum levels of aspartate transaminase, alanine transaminase, and liver index; while TG, DG in serum, and Co, LPS, PC in liver were negatively correlated with the parameters. In total, 43 and 34 lipid molecules were altered by taxifolin treatment in the liver and serum, respectively, mainly including glycerophosphoglycerols, glycerophosphocholines, glycerophosphoethanolamines, and linoleic acids and derivatives. Our findings help to provide novel insights into the mechanism of the hepatoprotective effect of taxifolin from a lipidomics approach.
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ANALYTICAL AND BIOANALYTICAL CHEMISTRY
·
2024
·Vol. 416
·期 29
·7043-7062
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IF 3.8
Liu Wen-Ya,Xu Di,Meng Hui-Hui,Wang Cheng-Yao,Feng Xin,Wang Jun-Song
Cucurbitacin B (CuB) is a natural triterpenoid with diverse pharmacological effects including potent anticancer activity. However, its oral bioavailability is hampered by limited metabolism in vivo. We characterized CuB’s in vivo metabolism in rats to uncover bioactive metabolites retaining therapeutic potential, using a robust UHPLC-Q-TOF–MS/MS workflow. This workflow combined molecular networking, fragmentation filtering, and mass defect filtering to identify CuB metabolites in rat urine, plasma, and feces following oral administration. Thirteen metabolites were identified and seven were confirmed. Major phase I transformations involved hydrolysis, reduction, epoxidation, and amination. Phase II conjugation included cysteine, glutathione, glucuronide, and gluconic acid conjugates. Notably, one of the main metabolites formed was the cysteine conjugate CuB-Cys. CuB-Cys maintained similar in vitro antiproliferative activity to CuB on HepG2, MCF-7, and PANC-1 cancer cell lines. However, it demonstrated lower cytotoxicity towards non-cancerous L02 cells, highlighting improved therapeutic selectivity. Mechanistically, CuB-Cys induced greater apoptotic signaling in HepG2 cells than CuB via enhanced caspase activation and disrupted BAX-Bcl-2 balance. This represents the first systematic characterization of CuB’s in vivo metabolic pathway. The identification and confirmation of CuB-Cys provide insight for drug development efforts aiming to maintain therapeutic efficacy while reducing toxicity, via metabolite-based approaches. Our findings shed light on strategies for improving CuB’s clinical potential. Graphical Abstract
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FOOD RESEARCH INTERNATIONAL
·
2026
·
IF 8.8
Yuanyuan Zhao,Yongmao Lu,Tian Yang,Shaohua Hu,Yuanyuan Yan,Xingguo Wang,Wei Wei
Multi-method strategy enhances accuracy in human milk vitamin research. • Mass spectrometry achieved precise 25(OH)D₂/₃ quantification in human milk. • Immunoassays offered rapid screening but showed a 72.98% positive bias. • Liquid chromatography profiled vitamins A and E but lacked sensitivity for D and K. • 25(OH)D₃ increased slightly, while 25(OH)D₂ declined across lactational stages. Accurate analysis of vitamin D in human milk is essential for infant nutrition but remains analytically challenging due to low levels and a complex matrix. This study evaluates a practical multi-method strategy using LC-MS/MS, ELISA, and UPLC-PDA for vitamin D analysis in human milk. LC-MS/MS precisely quantified 25(OH)D₂ and 25(OH)D₃ with assay LOQ of 0.045 ng/mL and 0.100 ng/mL, respectively. ELISA showed a 11.58 ng/mL positive bias of vitamin D which limits use for accurate quantification. UPLC-PDA profiled vitamins A and E effectively but lacked sensitivity for vitamin D. Longitudinally, LC-MS/MS results show 25(OH)D₃ and total 25(OH)D concentrations remained relatively stable, with medians ranging from 0.141 to 0.281 ng/mL and 0.263 to 0.315 ng/mL, respectively, across the study period, while 25(OH)D₂ peaked at 8 weeks before declining. This study establishes LC-MS/MS as the preferred analytical strategy for quantifying 25(OH)D 2 and 25(OH)D 3 in human milk, providing critical data to assess infant nutritional intake and guide clinical interventions. Download: Download high-res image (160KB) Download: Download full-size image
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JOURNAL OF SEPARATION SCIENCE
·
2019
·Vol. 42
·期 16
·2592-2601
·
IF 2.516
Hongmin Zhang,Xintong Hu,Miao Qiao,Yang Li,Shijie Cao,Liqin Ding,Xinchi Feng,Ning Kang,Deqin Zhang,Feng Qiu
A rapid and sensitive liquid chromatography with tandem mass spectrometry method was developed and validated for simultaneous determination of puerarin, daidzin, daidzein, 3′-hydroxy puerarin, and genistein in rat plasma after oral administration of Puerariae lobatae radix extract. The method of protein precipitation with acetonitrile was used for sample preparation. Chromatographic separation was achieved on a C 18 column with the mobile phases of acetonitrile/water containing 0.1% formic acid. The analytes were detected by mass spectrometer with an electrospray ionization source operating in the negative ion mode. The linearity, precision, accuracy, dilution reliability, recovery, matrix effects, and stability of the method were within acceptable ranges. The developed method was successfully used to compare the pharmacokinetic characteristics of five analytes in normal and type 2 diabetics rats after oral administration of Puerariae lobatae radix extract. Several pharmacokinetic alterations were observed and this might be caused by the pathological state of type 2 diabetes.
研究领域:
药理学
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分析化学
·
糖尿病研究
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FOOD CHEMISTRY
·
2023
·
IF 8.8
Youzhi Su,Jianjiang Lu,Jun Liu,Fang Li,Ning Wang,Hongqin Lei,Xiaofang Shen
A modified QuEChERS purification–liquid chromatography-tandem mass spectrometry method has been developed to determine 51 pesticide residues with newly established maximum residue limits (MRLs) in foodstuffs. Samples were extracted with acetonitrile under citrate-buffered conditions and purified using a modified QuEChERS method employing hydroxylated MWCNTs , SAX, and C 18 . The limits of quantification ranged from 0.2 to 9.8 µg/kg. Recoveries in ten different foodstuffs ranged from 70.2% to 117.9%, with relative standard deviations between 2.3% and 19.9% at three spiking levels. This method was applied to analyze 352 market samples, detecting 14 pesticides in 97 samples. Notably, Afidopyropen, cyantraniliprole, and fluxapyroxad residues in vegetables exhibited a consistent pattern of higher levels in the spring and winter and lower levels in the summer and autumn. Moreover, the risk assessments for acute and chronic dietary exposure to the 14 detected pesticides indicated that the %ADI and %ARfD were well below 100%.
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BULLETIN OF ENVIRONMENTAL CONTAMINATION AND TOXICOLOGY
·
2023
·Vol. 111
·期 4
·1-9
·
IF 2.7
Zheng Handinghong,Wu Qiong,Wu Xiaomao
This study aimed to investigate the dissipation, residues and dietary assessment of kresoxim-methyl in the application of Rosa Roxburghii and soil field using liquid chromatography-tandem mass spectrometry (LC–MS/MS). The results show that kresoxim-methyl in R. roxburghii samples was extracted by acetonitrile and purified by ethyl enediamine-N-propylsilane (PSA), while kresoxim-methyl in soil samples was extracted by acetonitrile and purified by octadecylsilyl solid phase dispersant (C 18 ). 0.1% formic acid (v/v)-water–methanol solution was used as the mobile phase, LC–MS/MS exhibited a good linearity in the range of 0.001–10 mg L −1 . The recoveries of R. roxburghii and soil matrix were 82.48%–102.55%, and the relative standard deviation ( RSD) were 1.13%–4.21%. The limit of detection ( LOD ) and quantification ( LOQ ) of kresoxim-methyl in R. roxburghii and soil samples was 0.50 and 0.60 µg kg −1 , respectively. The dissipation dynamics of kresoxim-methyl in R. roxburghii and soil followed the first-order kinetics, with the half-life of 4.28 and 4.41 days, respectively. The terminal residual amount of kresoxim-methyl in R. roxburghii and soil samples was 0.003–1.764 and 0.007–2.091 mg kg −1 , respectively. The dietary intake risk assessment indicates that a risk quotient ( RQ ) for kresoxim-methyl based on the national estimated daily intake ( NEDI ) of 0.1995 mg was 0.79%, suggesting that the use of kresoxim-methyl on R. roxburghii at recommended dosage was safe to consumers. This study provides the theoretical basis for guiding the rational use of kresoxim-methyl in the production of R. roxburghii .
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JOURNAL OF HAZARDOUS MATERIALS
·
2023
·
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.
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Marine Drugs
·
2023
·Vol. 21
·期 10
·502
·
IF 5.4
Yawen Wang,Longjian Zhou,Minqi Chen,Yayue Liu,Yu Yang,Tiantian Lu,Fangfang Ban,Xueqiong Hu,Zhongji Qian,Pengzhi Hong,Yi Zhang
The prevalence of gout and the adverse effects of current synthetic anti-gout drugs call for new natural and effective xanthine oxidase (XOD) inhibitors to target this disease. Based on our previous finding that an edible seaweedPterocladiella capillaceaextract inhibits XOD, XOD-inhibitory and anti-inflammatory activities were used to evaluate the anti-gout potential of differentP. capillaceaextract fractions. Through affinity ultrafiltration coupled with liquid chromatography tandem mass spectrometry (LC-MS/MS), feature-based molecular networking (FBMN), and database mining of multiple natural products, the extract’s bioactive components were traced and annotated. Through molecular docking and ADMET analysis, the possibility and drug-likeness of the annotated XOD inhibitors were predicted. The results showed that fractions F4, F6, F4-2, and F4-3 exhibited strong XOD inhibition activity, among which F4-3 reached an inhibition ratio of 77.96% ± 4.91% to XOD at a concentration of 0.14 mg/mL. In addition, theP. capillaceaextract and fractions also displayed anti-inflammatory activity. Affinity ultrafiltration LC-MS/MS analysis and molecular networking showed that out of the 20 annotated compounds, 8 compounds have been previously directly or indirectly reported from seaweeds, and 4 compounds have been reported to exhibit anti-gout activity. Molecular docking and ADMET showed that six seaweed-derived compounds can dock with the XOD activity pocket and follow the Lipinski drug-like rule. These results support the value of further investigatingP. capillaceaas part of the development of anti-gout drugs or related functional foods.Keywords:Pterocladiella capillacea;xanthine oxidase inhibitors;anti-inflammatory;affinity ultrafiltration LC-MS/MS;molecular networking
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危险品化学品经营许可证（带存储）