INTERNATIONAL JOURNAL OF BIOLOGICAL MACROMOLECULES
·
2018
·
IF 3.909
Baolei Fan,Tingting Li,Xiaofang Song,Chao Wu,Chunqi Qian
A specific HPLC-MS/MS (High-Performance Liquid Chromatography with tandem Mass Spectrometry) method was developed and validated for simultaneous determination of several monosaccharides in three kinds Osmanthus fragrans Lour . After extraction, separation, protein removal, pigment removal and hydrolysis , monosaccharides was finally obtained from Osmanthus fragrans Lour . Positive ion mode detection and Multiple Reaction Monitoring (MRM) mode were used for quantitative analysis by PMP pre-column derivatization and Electrospray Ionization (ESI). Analysis and content determination of 6 monosaccharide components in 3 kinds of Osmanthus fragrans Lour . The HPLC separation was achieved on a Shim-pack VP-ODS6022748 (150 L × 2.0) with gradient elution at a flow rate of 0.2 ml/min in a run time of 40 min, and the mobile phase was acetonitrile-5 mmol/L ammonium acetate. PMP derivatization in HPLC-MS/MS can accurately measure Osmanthus fragrans Lour . mannose (Man), ribose (Rib), rhamnose (Rha), galacturonic acid (Gal UA), glucose (Glu), galactose (Gal), xylose (Xyl), fucose (Fuc). The results showed that HPLC-MS/MS pre-column derivatization method was simple and rapid, with small measurement error, but high sensitivity and good repeatability. The analysis of monosaccharide components in polysaccharide components has important practical significance.
研究领域:
植物化学
·
分析化学
✓ 已验证
产品关联
DOI
PubMed
高影响因子
JOURNAL OF SEPARATION SCIENCE
·
2021
·Vol. 44
·期 9
·1852-1865
·
IF 3.645
Jingjing Wu,Song Zhang,Jiali Li,Xiaoli Zhong,Guiping Feng,Liangqing Hu,Fan He,Hanjing Cen,Yilu Chen,Yanling He,Huasong Zeng,Xiao Chen,Xiaolan Mo
Low-dose methotrexate is the first-line therapy for juvenile idiopathic arthritis. In vivo, methotrexate is converted into a series of methotrexate polyglutamates whose intracellular levels contribute significantly to its efficacy and toxicity. In this study, a novel high-performance liquid chromatography–tandem mass spectrometry method was developed and validated to simultaneously determine erythrocyte methotrexate polyglutamates using stable isotope-labeled internal standards. Erythrocyte samples were precipitated by perchloric acid and then determined on an XBridge BEH C18 column with an XP vanguard precolumn in 12 min. The mobile phase consisted of 10 nM ammonium acetate (pH 10) and methanol under gradient elution. The detection was carried out in multiple reaction monitoring mode via an electrospray ionization source in positive ionization mode. The calibration curve for each metabolite was linear from 2.0 to 500.0 nmol/L ( r 2 > 0.99). The intraday and interday accuracies were between 93.0 and 107.0%, and the corresponding precisions were between 0.8 and 5.2%. The relative recovery ranged from 82.7 to 105.1%, and the relative matrix effect varied from 96.5 to 104.4%. The erythrocyte metabolites were stable for 30 days at −80°C. This simple and accurate method is applicable to routine monitoring of the concentration of erythrocyte methotrexate polyglutamates in patients to achieve individualized treatment.
研究领域:
药理学
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分析化学
·
临床医学
✓ 已验证
DOI
PubMed
高影响因子
ACS Omega
·
2021
·
IF 3.512
Zhihui Lin,Yingnan Lin,Jianqi Lin,Yizhi Zhang,Song Fang
A modified QuEChERS method in combination with high-performance liquid chromatography-tandem mass spectrometry (HPLC-MS/MS) was first developed for the determination of fenbutatin oxide in six types of samples (soil, tobacco, rice, milk, pork liver, and pork). Fenbutatin oxide was extracted with acetonitrile containing 1% formic acid (v/v) and purified by dispersive solid-phase extraction using primary secondary amine (PSA) and quantitatively analyzed by HPLC-MS/MS. In the range of 0.005–1 mg/kg, a good linear relationship exists between the concentration of fenbutatin oxide and the peak area, giving a coefficient of determination (R2) of >0.99. The recoveries of fenbutatin oxide at three spiked levels were 79.04–97.12% with the relative standard deviations (RSDs) of 3.30–10.96%, and the limit of quantification (LOQ) was 0.007 mg/kg. In addition, the developed method is consistent with the reference method (R2 = 0.9896, n = 40). The method is demonstrated to be convenient and reliable for the routine monitoring of fenbutatin oxide in soil and plant- and animal-derived foods.
研究领域:
分析化学
·
食品安全
✓ 已验证
产品关联
DOI
PubMed
高影响因子
ANALYTICAL AND BIOANALYTICAL CHEMISTRY
·
2024
·
IF 3.8
Wu Jiaxin,Yao Shunying,Wang Yiwei,Fan Sai,Cui Xia,Chen Dawei,Shi Zhixiong
Organophosphate esters (OPEs) are commonly used chemicals and are also regarded as emerging environmental pollutants. Recently, it has been proved that metabolites of OPEs (mOPEs) could also cause health concerns. However, analytical methods for the concurrent measurement of OPEs and mOPEs in human matrices are still complicated. In this study, a convenient and efficient analytical method combining a cold-induced strategy and HPLC–MS/MS was developed to simultaneously determine 18 OPEs and 10 mOPEs in human serum, urine, and human milk. In brief, after the sample was extracted with acetonitrile, a “one-step” treatment combining purification and enrichment was accomplished by cold-induced liquid–liquid extraction (CI-LLE), and analytes were then quantified by HPLC–ESI–MS/MS. The ratio of acetonitrile/water, and the temperature and time set in the CI-LLE procedure were optimized for achieving the highest enrichment factors. Under the best conditions, linearity, limits of detection (LODs), recovery, precision, and matrix effects of OPEs/mOPEs were verified. LODs of OPEs/mOPEs in serum, urine, and human milk were 0.1–113 pg/mL, 0.1–22 pg/mL, and 0.2–22 pg/mL, respectively. Average recoveries ranged from 80 to 123%, with relative standard deviations lower than 15% for most analytes. The matrix effect test showed slight signal enhancement or inhibition, and the use of isotopically labeled internal standards (ISs) could compensate for the effects. In real sample analysis, both OPEs and mOPEs showed high detecting frequency, which indicated their ubiquity in humans.
研究领域:
环境科学
·
分析化学
·
毒理学
✓ 已验证
产品关联
DOI
PubMed
高影响因子
TALANTA
·
2025
·
IF 6.1
Zheng Hu,Yuhang Yang,Zhe Li,Qiuying Tao,Yinghong Huang,Xian Wang
Endocrine-disrupting chemicals (EDCs) are a growing class of pollutants commonly found in environmental matrices due to their extensive use in pharmaceuticals and personal care products (PPCPs). In this study, a novel magnetic covalent organic framework (COF), Fe 3 O 4 –COOH@TFP-BHBD, was successfully synthesized and utilized as an adsorbent for magnetic solid-phase extraction (MSPE) of EDCs from PPCPs. The core-shell structured adsorbent demonstrated a high specific surface area, strong magnetic responsiveness and excellent stability. A COF-MSPE-high-performance liquid chromatography-tandem mass spectrometry (COF-MSPE-HPLC-MS/MS) method was developed for the quantitative analysis of EDCs in PPCPs. Under the optimized condition, the detection and quantification limits of this method reached as low as 0.001–0.007 ng/mL and 0.004–0.025 ng/mL, respectively. This method was validated and proven capable to analyze real PPCP samples, while the spiked recovery rates in ranged from 85.62 to 107.83 % with RSD of 2.28–8.58 %. Moreover, the adsorption mechanism was investigated using density functional theory (DFT) calculations. The DFT results revealed that the efficient enrichment capacity of Fe 3 O 4 –COOH@TFP-BHBD for EDCs can be attributed to π-π interactions and hydrogen bondings. This proposed method provides excellent adsorption ability and sensitivity for the extraction and precise detection of EDCs in PPCPs.
研究领域:
环境科学
·
分析化学
✓ 已验证
产品关联
DOI
PubMed
高影响因子
Canadian Journal of Chemistry
·
2013
·Vol. 91
·期 11
·
IF 0.964
ChenMiao,LiuLiangliang,ChenXiaoqing
Alcohol dehydrogenase (ADH) is a key enzyme that converts ethanol into acetaldehyde. Its binders could be used to efficiently treat human toxic alcohol poisoning and suppress the acetaldehyde accumulation in alcohol hypersensitive alcoholics. In the present study, a new assay based on ADH-functionalized magnetic nanoparticles coupled with high-performance liquid chromatography − tandem mass spectrometry (HPLC−MS/MS) was developed for the rapid screening and identification of ADH binders. ADH was immobilized on silica-coated Fe3O4 magnetic nanoparticles via covalent bonds and the synthesized nanoparticles were characterized by TEM, XRD, FT-IR, and VSM. The amount of bound ADH onto magnetic nanoparticles was 80.6 μg/mg. The optimum temperature and pH for the enzymatic activity of immobilized ADH were 25 °C and 7.0, respectively. The relative activity of immobilized ADH remained 68.14% after 10 times of recycle, which exhibited good durability. Nine compounds with ADH-binding activity were screened and identified in Glycyrrhiza uralensis root extracts, among which seven compounds were first screened and identified. Experimental results proved that the proposed method could rapidly screen ADH binders from complex mixtures.
研究领域:
生物化学
·
药物开发
·
分析化学
✓ 已验证
DOI
高影响因子
ANALYTICAL LETTERS
·
2022
·
IF 2.267
Ru Li,Xuan Zou,Pan Luan,Xiaokun Liu,Ning Wang,Qian Wang,Huashi Guan,Zhe Xu
Thrombosis is the main cause of many cardiovascular diseases. The conventional pharmaceuticals used for preventing thrombosis can induce significant adverse side effects, especially bleeding risk. Hence, the development of more effective and safe antithrombotic agents is strongly demanded to improve clinical treatment. In order to rapidly screen and identify novel antithrombotic substances from natural marine products, a multi-target screening strategy is reported to quantify the antithrombotic activity with high-performance liquid chromatography – mass spectrometry (HPLC-MS). Five key thrombosis-related targets, including thrombin, coagulation factors Xa, XIa and XIIa and platelet phosphodiesterase 3, were selected to establish the multi-target antithrombotic activity screening assay. The Michaelis-Menten constants (Km) were 8.16 µM, 58.85 µM, 120.03 µM, 35.24 µM and 79.67 µM, respectively. Five known inhibitors, namely argatroban, rivaroxaban, benzamidine, 3-carboxamide-coumarinand, and milrinone, were used for validation. The reproducibility of the screening strategy was verified by calculating the overall average Z′ value, which was 0.88. Subsequently, this method was assessed by screening a small marine library of 78 compounds. Five coumarin compounds were selected, and their antithrombotic activities were further validated in standard assessments of enzyme inhibition and on the coagulometer. According to the validation, the multi-target assay based on dried blood spots and HPLC-MS was suitable for screening antithrombotic substances with considerable reliability.
研究领域:
药理学
·
分析化学
·
心血管病学
✓ 已验证
产品关联
DOI
高影响因子
MICROCHEMICAL JOURNAL
·
2019
·
IF 3.206
Hui Guo,Yunfei Chen,Na Song,Xinyi Yang,Shen Yao,Junqing Qian
Bamboo leaf is known as dietic tea for the prevention of obesity in China. To screen lipase inhibitors from bamboo leaf extract rapidly, lipase functionalized magnetic ligand fishing combined with HPLC/MS was established. Firstly, lipase was immobilized on magnetic nanoparticles by dialdehyde starch to obtain lipase-functionalized magnetic nanoparticles (L-MNPs), and then the L-MNPs were incubated with bamboo leaf extract to fish out ligands. Three enzyme inhibitors were obtained and identified as isoorientin, orientin, isovitexin by HPLC/MS. The results provided a powerful evidence for explaining the hypolipidemic effects of bamboo leaf extract, and this ligand fishing method is feasible for screening enzyme inhibitors from complex mixtures.
研究领域:
生物化学
·
药物筛选
·
食品科学
✓ 已验证
产品关联
DOI
高影响因子
MICROCHEMICAL JOURNAL
·
2020
·
IF 3.594
Baolei Fan,Guoliang Wei,Xiaofeng Gan,Tingting Li,Zengyi Qu,Sheng Xu,Chao Liu,Chunqi Qian
In this study, we reported the various contents of Polygonatum cyrtonema by extracting polysaccharides (PCPs) using steaming and shining procedures, thus providing scientific basis for the processing of Polygonatum cyrtonema and content analysis of polysaccharides. We established the characteristic fingerprint to identify and analyze polysaccharide component changes in distillated and processed Polygonatum cyrtonema by PMP precolumn derivatization and HPLC-MS/MS technology. We also classified two kinds of solutions by comparing the composition difference of 10 polysaccharide components in the samples with principal component and cluster analysis. There was a huge difference between them and seven monosaccharides. Processed PCPs mainly consisted of galactose along with mannose, followed by glucose. Meanwhile, we found that the results of cluster analysis and principal component analysis were the same. The polysaccharide components extracted from processed Polygonatum cyrtonema and distillate were mainly galactose and mannose. The results of cluster analysis and principal component analysis were the same. The distilled liquid can be divided into 5 categories, and the processed dry extract of Polygonatum cyrtonema can be divided into 4 categories. The changing trend of polysaccharide components of Polygonatum cyrtonema and distilled liquid was revealed during the multiple cycles of steaming and sun drying. The similarity and difference of polysaccharide components in the extracted liquid and the distilled liquid of each batch were shown.
研究领域:
中药学
·
分析化学
·
植物化学
✓ 已验证
产品关联
DOI
高影响因子
FOOD CHEMISTRY
·
2025
·
IF 9.8
Yupeng Wen,Wendi Huo,Xinyuan Zhang,Yingchun Mu,Huan Liu,Chaoying Zhang,Lu Qiao,Jincheng Li
In this study, we developed a miniaturized semi-automatic purification method based on pressure-filtration purification for sensitive HPLC-MS/MS monitoring of pesticides in aquatic products. For the first time, loofah sponge was demonstrated and utilized as a novel green, low-cost, and effective one-step purification adsorbent for fish sample. The developed method consisted of two main steps: first, target analytes were extracted from fish samples using an acetonitrile-based QuEChERS extraction method. Subsequently, the extract was automatically purified through a pressure-filtration purification column in a centrifuge, followed by HPLC-MS/MS analysis. Under optimized experimental conditions, the method exhibited excellent linearity, with a range of 1.0 to 50.0 μg/kg and a correlation coefficient > 0.99. The detection and quantification limits were 0.5 and 1–2 μg/kg, respectively. Recoveries at spiked levels of 2.0, 5.0 and 30.0 μg/kg ranged from 69.95 to 104.88 %, with intra-day RSDs ranging from 0.58 to 15.01 % and inter-day RSDs ranging from 0.72 % to 14.32 %.
研究领域:
食品科学
·
环境科学
·
分析化学
✓ 已验证
产品关联
DOI
PubMed
高影响因子
Pharmaceuticals
·
2021
·Vol. 14
·期 11
·1194
·
IF 5.863
Min Li,Qingfeng He,Li Yao,Xiaofeng Wang,Zhijia Tang,Xiao Zhu,Hai-Shu Lin,Xiaoqiang Xiang
Propylthiouracil (PTU) is commonly prescribed for the management of hyperthyroidism and thyrotoxicosis. Although the exact mechanism of action is not fully understood, PTU is associated with hepatoxicity in pediatric population. Glucuronidation mediated by uridine 5′-diphospho-glucuronosyltransferases (UGTs), which possess age-dependent expression, has been proposed as an important metabolic pathway of PTU. To further examine the metabolism of PTU, a reliable HPLC-MS/MS method for the simultaneous quantification of PTU and its N-β-D glucuronide (PTU-GLU) was developed and validated. The chromatographic separation was achieved on a ZORBAX Extend-C18 column (2.1 × 50 mm, 1.8 μm) through gradient delivery of a mixture of formic acid, methanol and acetonitrile. The electrospray ionization (ESI) was operated in its negative ion mode while PTU and PTU-GLU were detected by multiple reaction monitoring (MRM). This analytical method displayed excellent linearity, sensitivity, accuracy, precision, recovery and stability while its matrix effect and carry-over were insignificant. Subsequently, the in vitro metabolism of PTU was assessed and UGT1A9 was identified as an important UGT isoform responsible for the glucuronidation of PTU. The information obtained from this study will facilitate future mechanistic investigation on the hepatoxicity of PTU and may optimize its clinical application.Keywords:propylthiouracil;propylthiouracil glucuronide;in vitro;human liver microsomes;UGT1A9;HPLC-MS/MS
研究领域:
药理学
·
分析化学
·
毒理学
✓ 已验证
产品关联
DOI
PubMed
高影响因子
ANALYST
·
2014
·Vol. 139
·期 23
·6168-6177
·
IF 3.906
Ruifang Qi,Xiao Zhou,Xiqian Li,Jiutong Ma,Chunmei Lu,Jun Mu,Xuguang Zhang,Qiong Jia
A synthetic protocol for the preparation of an indium oxide nanoparticle-functionalized poly(methacrylic acid-glycidyl methacrylate-ethylene dimethacrylate-ethanediamine) monolithic column is reported. Various techniques, including scanning electron microscopy, transmission electron microscopy, Fourier transform infrared spectroscopy, X-ray photoelectron spectroscopy, and thermal gravimetric analysis-derivative thermogravimetric analysis were employed to characterize the synthesized monolith. The modified monolithic column was coupled with high performance liquid chromatography-tandem mass spectrometry (HPLC-MS/MS) for determining synthetic colorants in various food samples. Under optimized conditions, good linearity was obtained for all the targets with squared regression coefficients greater than 0.9982. The limits of detection (S/N = 3) for 12 synthetic colorants were in the range of 0.012–2.97 μg kg−1. The intra-day and inter-day relative standard deviations, ranging from 2.7% to 8.5%, were within the acceptable range. The developed method was successfully applied to the determination of synthetic colorants in food samples (candy, milk, jelly, jam, canned food, juice, and carbonated drink). Target recoveries at different spiked levels ranged from 73.5% to 112.1% with relative standard deviations of less than 10.3%.
研究领域:
分析化学
·
食品安全
✓ 已验证
DOI
PubMed
高影响因子
危险品化学品经营许可证（带存储）