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
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药物开发
·
分析化学
✓ 已验证
DOI
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
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
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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
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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
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分析化学
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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
Frontiers in Environmental Science
·
2022
·
IF 5.411
Wang Siwei,Sun Haibin,Liu Yanping,Wang Xiaonan,Chang Hong
A modified-QuEChERS method to determine kresoxim-methyl in banana and soil was developed and validated via high-performance liquid chromatography–tandem mass spectrometry (HPLC-MS/MS). The dissipation behavior, residue distribution, and risk assessment of kresoxim-methyl in banana were further investigated based on this method. The dissipation behavior of kresoxim-methyl in banana and soil was described by using first-order kinetics and its half-life, 4.8–5.7 days and 5.5–6.5 days, respectively. The concentrations of kresoxim-methyl were 0.03–0.08 mg kg−1, 0.06–0.17 mg kg−1, and <0.01 mg kg−1 for a whole banana, peel, and pulp, respectively, on the basis of spraying three times the recommended dosage and pre-harvest interval (PHI, 42 days). The results showed that the risk quotient of kresoxim-methyl in banana to people exhibited an acceptable low dietary risk. This current study could help in guiding the scientific and proper usage of this formulation.
研究领域:
农业化学
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食品科学
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环境科学
✓ 已验证
产品关联
DOI
高影响因子
Analytical Methods
·
2016
·Vol. 8
·期 6
·1405-1414
·
IF 1.915
Na Cao,Lei Liu,Yuan-bin Hao,Li-li Sun,Qiao-gen Zou,Xing-ling Ma,Kai-he Xiong
A sensitive, rapid and stable HPLC-MS/MS method has been developed and validated for the determination of rabeprazole enantiomers and their four metabolites, namely rabeprazole thioether, rabeprazole sulfone and desmethyl rabeprazole enantiomers, in beagle dog plasma using esomeprazole as the internal standard. The analytes and the internal standard were extracted from plasma samples by liquid–liquid extraction and separated on a Chiral-HSA column using acetonitrile-10 mmol L−1 ammonium acetate as the mobile phase by gradient elution. The method was validated with respect to sensitivity, specificity, linearity, precision, accuracy and especially the stability of analytes under various conditions, and was successfully applied in evaluating the pharmacokinetic profiles of racemic rabeprazole, the pure enantiomers and their metabolites in beagle dogs after single intravenous administration of (R)-rabeprazole sodium injection (at 0.33, 1 and 3 mg kg−1), (S)-rabeprazole sodium injection (at 1 mg kg−1) and racemic rabeprazole sodium injection (at 2 mg kg−1). The two enantiomers showed different profiles of pharmacokinetic parameters. The AUC0–t and t1/2 values of (R)-rabeprazole were higher and the clearance (CL) value of (R)-rabeprazole was lower than that of (S)-rabeprazole. Compared to (S)-rabeprazole, the higher absorption and slower elimination of (R)-rabeprazole explain why (R)-rabeprazole is more effective than the racemate.
研究领域:
药物分析
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药理学
·
临床医学
✓ 已验证
产品关联
DOI
高影响因子
MICROCHEMICAL JOURNAL
·
2021
·
IF 4.821
Fukai Li,Min Wang,Jian Zhou,MengRui Yang,TongTong Wang
A novel cyclodextrin-derivatized hybrid magnetic nanocomposite, denoted as Fe 3 O 4 @SiO 2 @CD, was fabricated and employed as the adsorbent of magnetic solid-phase extraction (MSPE) for preconcentration of elven fluoroquinolones (FQs) from water samples. The prepared nanoparticles exhibited excellent magnetic responsiveness (56.7 emu g −1 ), uniform size distribution (about 300 nm), good thermal and chemical stability, excellent reusability and superior chemical affinities to the target FQs via hydrogen bond, host–guest inclusion complexation and π–π interactions. Under the optimized conditions, the MSPE was coupled with HPLC-MS/MS to sensitively quantify trance levels of FQs in environmental water. The developed method revealed satisfactory precision with RSDs lower than 4%, good linearity (R 2 ≥ 0.9981), low limits of detection (0.0014–0.023 µg L −1 ) and satisfactory recoveries (93.2–105%). Furthermore, the proposed approach was validated by analyzing the Certified Reference Material of GBW 10152 and GBW 10153 chicken meat powder. These results demonstrated that the Fe 3 O 4 @SiO 2 @CD nanoparticles are a promising magnetic adsorbent for FQs, and the established MSPE-HPLC-MS/MS approach is suitable for simultaneous analysis of trace levels of FQs in actual samples.
研究领域:
分析化学
·
环境科学
·
药物分析
✓ 已验证
产品关联
DOI
高影响因子
FOOD CHEMISTRY
·
2024
·
IF 8.5
Ruidong Zhou,Yupeng Wen,Wendi Huo,Cong Kong,Guangxin Yang,Huan Liu,Chaoying Zhang,Yingchun Mu,Dongmei Huang,Jincheng Li
A modified QuEChERS method was developed to determine multi-class pesticide and veterinary residues in aquatic products. Chitosan microspheres were conveniently synthesized and utilized as the cleanup adsorbent in the QuEChERS procedure, showcasing rapid filtration one-step pretreatment ability for the determination of drug multi-residues in aquatic products. Compared to conventional synthetic sorbents, chitosan microspheres not only have good purification performance, but also have renewable and degradable properties. This novel sorbent worked well in the simultaneous determination of 95 pesticides and veterinary drug residues in aquatic products after being combined with an improved one-step vortex oscillating cleanup method. We achieved recoveries ranging from 64.0% to 115.9% for target drugs in shrimp and fish matrix. The limits of detection and quantification were 0.5–1.0 and 1.0–2.0 μg kg −1 , respectively. Notably, hydrocortisone was detected with considerable frequency and concentration in the tested samples, underscoring the necessity for stringent monitoring of this compound in aquatic products.
研究领域:
分析化学
·
环境科学
·
食品安全
✓ 已验证
产品关联
DOI
PubMed
高影响因子
MICROCHIMICA ACTA
·
2018
·Vol. 185
·期 3
·1-9
·
IF 5.705
Ji Shunli,Li Tengfei,Yang Wen,Shu Chang,Li Duo,Wang Yan,Ding Li
A hollow porous molecularly imprinted polymer (HPMIP) is described for use in dispersive solid phase extraction of macrolide antibiotics (MACs). The HPMIP was prepared by using spiramycin as the template, methacrylic acid as the functional monomer, and mesoporous MCM-41 (Mobile Composition of Matter No. 41; with a size of about 100 nm) as a sacrificial support. The sorbent was characterized by Fourier transform infrared spectrometry, transmission electron microscopy, nitrogen adsorption and thermo-gravimetric analysis. Several parameters affecting the extraction efficiency were optimized. The material has a large surface area (359 m 2 ·g −1 ), and most recognition sites are located on the surface of the HPMIPs. This results in high binding capacity (120 μmol·g −1 ) and fast binding (20 min) in comparison to either MCM-41-core surface MIPs or solid MIPs. The method was applied to the extraction of the MACs azithromycin, spiramycin, tilmicosin, tylosin, clarithromycin, roxithromycin and josamycin from spiked honey. The recoveries, determined by HPLC-MS/MS, ranged from 88.0% to 117% at the three spiking levels tested (1, 5 and 20 μg·kg −1 ). Intra-day and inter-day assay precision at three spiking levels are <10.7% (for n = 6) and 12.6% ( n = 3), respectively. The limits of detection are between 3 and 17 ng·kg −1 . This indicates the superiority of the method in selective extraction of macrolides even from complex matrices.
Hollow porous molecularly imprinted polymers using spiramycin as the template are shown to be viable dispersive solid phase extraction adsorbents for selective enrichment of macrolide antibiotics in honey products prior to their quantitation by HPLC-MS/MS.
研究领域:
分析化学
·
食品科学
✓ 已验证
DOI
PubMed
高影响因子
Journal of Pharmaceutical Analysis
·
2020
·
IF 2.673
Yuan Hong,Xiaoyan Liao,Zilin Chen
The fruits of leguminous plants Cercis Chinensis Bunge are still overlooked although they have been reported to be antioxidative because of the limited information on the phytochemicals of C. chinensis fruits. A simple, rapid and sensitive HPLC-MS/MS method was developed for the identification and quantitation of the major bioactive components in C. chinensis fruits. Eighteen polyphenols were identified, which are first reported in C. chinensis fruits. Moreover, ten components were simultaneously quantified. The validated quantitative method was proved to be sensitive, reproducible and accurate. Then, it was applied to analyze batches of C. chinensis fruits from different phytomorph and areas. The principal components analysis (PCA) realized visualization and reduction of data set dimension while the hierarchical cluster analysis (HCA) indicated that the content of phenolic acids or all ten components might be used to differentiate C. chinensis fruits of different phytomorph.
研究领域:
药用植物学
·
分析化学
·
植物科学
✓ 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）