JOURNAL OF PHARMACEUTICAL AND BIOMEDICAL ANALYSIS
·
2020
·
IF 3.209
Youxi Jin,Yu Pan,Biao Jin,Dongri Jin,Chunbo Zhang
(S)-1-(5-(4-Methylpiperazin-1-yl)-2,4-dinitrophenyl)pyrrolidine-2-carboxylic acid (Pro-PPZ) was employed as a chiral derivatization reagent (CDR) for the efficient enantioseparation and ultrasensitive mass spectrometric detection of chiral amines. Pro-PPZ was prepared from the one-step reaction of 1-(5-fluoro-2,4-dinitrophenyl)-4-methylpiperazine (PPZ) and l -proline. Two amines and two amino acid methyl esters were selected as model chiral amines, which were easily labeled with Pro-PPZ under mild reaction conditions (35 °C for 10 min) generating Pro-PPZ-amine derivatives. The resulting diastereomers were completely separated by reversed-phase liquid chromatography (RP-LC) using an ODS column ( R s = 3.4–17.0 for amines). Ultrasensitive detection limits on femtomolar level were obtained for the tested amines using multiple reaction monitoring (MRM) chromatograms at a single monitoring ion, m/z 289 (0.1–5.0 fmol for amines). The practical metabolite analysis of (R)-1-aminoindan (R-AI) in saliva samples was performed by LC–MS/MS using the Pro-PPZ derivatization method. The method was validated in terms of precision, accuracy, and linearity. Using this method, R-AI concentrations in saliva were determined after a single oral administration of the drug rasagiline to healthy male and female subjects, but no (S)-1-aminoindan (S-AI) was detected, which suggesting that R-AI was not converted into S-enantiomer in the metabolic process. R-AI concentrations in four healthy volunteers ranged from 32.85 nM to 49.45 nM, with an average value of 43.76 nM. To date, there is no LC–MS (or MS/MS) method reported for the enantioselective determination of R-AI in human saliva samples.
研究领域:
分析化学
·
药物代谢
·
临床医学
✓ 已验证
DOI
高影响因子
MICROCHEMICAL JOURNAL
·
2024
·
IF 4.9
Xiao-Kang Fu,Si-Qi Han,Xiao-Bo Zhao,Jing-Yan Kang,Wei Ha,Yan-Ping Shi
Steroid hormone residues in food are a significant sources of endocrine disrupting chemicals (EDCs) that can adversely affect public health. However, the current analytical methods for determining steroid hormones using liquid chromatography-tandem mass spectrometry (LC-MS/MS) can be challenging due to the poor ionization efficiency of steroid hormones and the matrix effect of complex food samples. Herein, based on Cu(I)-catalyzed azide-alkyne cycloaddition (CuAAC) reaction and stable isotope labeling (SIL) technique, a novel pair of chemoselective probes ABI / d 5 -ABI was precisely designed and synthesized. This pair of probes comprises a H/D isotope tag, a linker, a reactive site azido group (N 3 ) and a MS tag (imidazolium salt). The probe ABI was employed to label ethynyl-containing steroid hormones in real samples and d 5 -ABI was applied to label standards, respectively, followed by mixing the two labeled samples for high performance (HP)LC-MS/MS analysis. It was found that the ionization efficiencies of target analytes were increased by 17–4532 folds after ABI labeling. More importantly, the heavy labeled samples serving as internal standards (ISs) can effectively compensate matrix effect during HPLC-MS/MS analysis. Finally, the proposed SIL-HPLC-MS/MS method was successfully used to highly sensitive determine four synthetic steroid hormones in food samples (milk, pork and egg). Furthermore, the good detection limits (0.015–0.020 ng/mL), satisfactory recoveries (75.7–122.9 %), and precisions (RSDs less than 9.2 %) were obtained. Hence, the established method not only provides new insights in designing SIL probes for determination of ethynyl-containing analytes within complex matrix, but also extends the application of CuAAC reaction in the field of food chemistry.
研究领域:
分析化学
·
食品科学
·
质谱技术
✓ 已验证
产品关联
DOI
高影响因子
LWT-FOOD SCIENCE AND TECHNOLOGY
·
2024
·
IF 6
Dan Wei,Qiao Deng,Jianliang Li,Jingjing Xu,Ming Guo,Huizhen Wu,Ju Zhang,Jianchang Jin,Xu Wang
Mycotoxins co-contamination in soybean poses great risks to human health, however, due to their diverse structures, it is difficult to simultaneously extract and detect these multi-mycotoxins. By incorporating modification of hydrophilic carboxyl groups with the hydrophobic properties of covalent organic frameworks, a stable cubic carboxyl-functionalized magnetic amide-linked covalent organic framework were fabricated, characterized and utilized as adsorbents for magnetic solid phase extraction (MSPE) of eleven frequently detected mycotoxins from soybeans followed by HPLC-MS/MS analysis. The key MSPE parameters were screened using the Plackett-Burman design and optimized with the Box-Behnken design for response surface methodologies. Under the optimal experimental conditions, the linear range was 0.2–50 μg/kg, the limits of detection were 0.1–1.4 μg/kg. The established method was applied for the soybean analysis with satisfactory recoveries (70.8–108.3%) and precision (intra- and inter-relative standard deviations of 2.1–9.2% and 1.6–11.1%, respectively). With proper modification, this method may have great application potential for simultaneously analyzing and monitoring the multi-mycotoxin contamination in foods to ensure consumer safety and public health.
研究领域:
分析化学
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食品科学
·
毒理学
✓ 已验证
产品关联
DOI
高影响因子
JOURNAL OF CHROMATOGRAPHY A
·
2024
·
IF 3.8
Jiaming Yuan,Jincai Wang,Zhixu Chen,Yuexiang Chang,Litong Chen,Zhizeng Gao,Jacques Crommen,Tingting Zhang,Zhengjin Jiang
In this study, a novel at-line nanofractionation platform was established for screening SARS-CoV-2 fusion inhibitors from natural products for the first time by combining HPLC-MS/MS with high-throughput fluorescence polarization (FP) bioassay. A time-course FP bioassay in 384 well-plates was conducted in parallel with MS/MS to simultaneously obtain chemical and biological information of potential fusion inhibitors in Lonicerae Japonicae Flos (LJF) and Lianhua Qingwen capsules (LHQW). Semi-preparative liquid chromatography and orthogonal HPLC separation were employed to enrich and better identify the co-eluted components. After comprehensive evaluation and validation, 28 potential SARS-CoV-2 fusion inhibitors were screened out and identified. Several compounds at low micromolar activity were validated by in vitro inhibitory assay, molecular docking, cytotoxicity test, and pseudovirus assay. Moreover, four potential dual-target inhibitors against influenza and COVID-19 were discovered from LJF using this method, offering novel insights for the development of future pharmaceuticals targeting epidemic respiratory diseases.
研究领域:
药学
·
分析化学
·
病毒学
·
药物发现
✓ 已验证
产品关联
DOI
PubMed
高影响因子
MICROCHEMICAL JOURNAL
·
2025
·
IF 5.1
Huiyu He,Rui Wang,Rongbin Nie,Nan Dong
Trace amounts of pharmaceuticals and personal care products (PPCPs) in aquatic environment poses a non-negligible risk to human health. Here, an environmentally friendly cucurbit[7]uril-mediated magnetic-assisted matrix solid phase dispersion (Q[7]- m -MSPD) extraction method was developed for extracting PPCPs from complex aquatic organisms. The extraction of PPCPs were achieved via the host-guest interaction between Q[7] and targets, significantly reducing the matrix interference. Gold magnetic nanoparticles (AuMNPs) were chelated to Q[7]-target complexes and used for purification and enrichment via magnetic solid-phase extraction (MSPE), effectively replacing the complex operation of sample loading and elution on SPE columns in MSPD. Coupled with high performance liquid chromatography-tandem mass spectrometry, multiple analysis of 14 PPCPs in 3 aquatic plants and an aquatic animal were achieved, with detection limits ranging from 0.0015 to 0.0179 μg/kg, recoveries ranging from 71.06 to 113.6 %, and enrichment factors within 46 to 152. The green chemistry assessment confirmed the environmental friendliness, economic feasibility, and application potential of the Q[7]- m -MSPD, with an AGREE score of 0.63 and a BAGI score of 72.5. By integrating the merits of MSPD and MSPE, the proposed approach exhibited high sensitivity and anti-interference capability, simple operation, and great environmental friendliness. Therefore, the approach provided a green method for simultaneously detecting multiple hazardous residues in complex matrices owing to the broad-spectrum molecular recognition capability of Q[7] , which has a good application prospect in food safety and environmental monitoring.
研究领域:
分析化学
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环境科学
·
绿色化学
·
食品安全
·
药物分析
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生物分析化学
✓ 已验证
产品关联
DOI
高影响因子
FOOD CHEMISTRY
·
2015
·
IF 3.391
Xiangyu Sun,Xueyin Li,Peiyue Wang,Tingting Ma,Weidong Huang,Shen Han,Jicheng Zhan
A new detection method of natamycin via HPLC–MS/MS was developed that uses an Agilent 6460 HPLC–MS/MS instrument and an Agilent RP18 (2.1 mm × 50 mm, 1.8 μm); the LOD was 1 μg/L, the LOQ was 3.34 μg/L, the recovery was 70–94%, the RSD was approximately 2–4%, and the total run time was 5 min. In the new detection method of natamycin via HPLC–MS/MS, processing of the sample before detection is necessary, which can be performed using solid phase extraction. Surprisingly, natamycin was not detected in any the sampled retail commercial wines from the Chinese market. Natamycin is very unstable in wine because many process steps, including the malo-lactic fermentation, clarification and storage, could result in degradation of natamycin. Regarding the clarifying agents, bentonite exhibited the strongest effect on natamycin. During the storage period, natamycin is very sensitive to light.
研究领域:
食品科学
·
分析化学
✓ 已验证
产品关联
DOI
PubMed
高影响因子
Antibiotics-Basel
·
2022
·Vol. 11
·期 10
·1427
·
IF 5.222
Hongli Ye,Siman Li,Yinfeng Xi,Yongfu Shi,Xiaorui Shang,Dongmei Huang
Antibiotic drug residues are crucial to ensure food safety and minimize risk to human health. Herein, a sensitive high-performance liquid chromatography–tandem mass spectrometry (HPLC–MS/MS) method was developed and validated for the determination of antibiotic residues (mainly amphenicols) consisting of chloramphenicol (CAP), thiamphenicol (TAP), florfenicol (FF), and florfenicol amine (FFA) in aquatic products. Amphenicols were well separated on a Kinetex F5 (100 mm × 3.0 mm, 2.6 µm) chromatographic column with the mobile phases of 1 mM ammonium acetate aqueous solution and methanol solution and measured after positive and negative electrospray ionizations using four internal standards. To our knowledge, it was the first time to report the good performance of F5 column and four internal standards for the determination of amphenicols. The established method featured a good linear relationship between chromatographic peak area ratios and the concentrations of amphenicols (R2> 0.992), a wide and low detection matrix-based range of 0.01–5 μg/L, a low detection limit of 0.01 μg/kg, etc. The spiked assays evidenced the accuracy and reliability of the developed method with the recoveries between 84.0 and 105%, the intraday relative standard deviations (RSDs) over the range of 0.769–13.7%, and the interday RSDs over the range of 0.582–13.3%. Finally, the proposed method was applied to investigate amphenicol residues in various aquatic products, including fish, shrimp, crab, shellfish, and other aquatic species.Keywords:antibiotics;amphenicols;detection;sensitivity;aquatic products;HPLC–MS/MS
研究领域:
食品安全
·
分析化学
·
环境科学
✓ 已验证
产品关联
DOI
PubMed
高影响因子
Natural Product Communications
·
2023
·
IF 1.8
Qing Xu,Dekun Li,Meixu Wan,Yanxin Zhang,Zhi Li,Aichun Ju
ObjectiveIn this study, an online CMC–LC/MS method was established in order to screen the active components of Yiqi Fumai lyophilization injection (YQFM) related to angiogenesis. The pro-angiogenic active components of YQFM were screened using this system and were then further verified.MethodsThe ECV304/CMC model coupled online with an HPLC–MS system was initially developed to screen, analyze, and identify the allergenic components of YQFM. A fraction was retained on the ECV304/CMC column, which was identified as ginsenoside Rb2. A cell proliferation assay and zebrafish intestinal microvascular model labeled with green fluorescence were used to detect the proliferation effect of ginsenoside Rb2.Results(1) The active component in YQFM, which was retained on the column, was ginsenoside Rb2. (2) Within a concentration range of 2.5–20 μg/mL, ginsenoside Rb2 was shown to promote the proliferation of ECV304 and EPCs cells and increase the area of sub-intestinal vessels in zebrafish.ConclusionGinsenoside Rb2, the active component in YQFM, can promote angiogenesis. The ECV304/CMC-online-HPLC system may serve as an effective screening tool for the vasoactive components from the traditional Chinese medicine injection.
研究领域:
药理学
·
中药学
·
分子生物学
✓ 已验证
产品关联
DOI
高影响因子
MOLECULES
·
2018
·Vol. 23
·期 7
·1804
·
IF 3.098
Xiao Chen,Jia Xiong,Lingxiao He,Yu Zhang,Xun Li,Liping Zhang,Fei Wang
The stability and bioaccessibility of polyphenol fromAcacia mearnsiibark were measured at various stages during in vitro simulated digestion. Subsequently, the changes in the total polyphenol content (TPC) and biological activity were studied. The results showed that the phenolic compounds fromA. mearnsiiremained stable, and TPC underwent few changes during gastric digestion. Nonetheless, intestinal digestion led to the degradation of proanthocyanidins (PAs) and a significant decrease in TPC (26%). Degradation was determined by normal-phase HPLC and gel permeation chromatography. Only monomers, dimers, and trimers of flavan-3-ols were identified in the serum-accessible fraction for characterization of their bioaccessibility. The results also indicated the obvious antioxidant capacity of PAs fromA. mearnsiibark, and ~53% of the α-glucosidase–inhibitory effect was preserved. All these findings show that PAs fromA. mearnsiibark as a native plant source may be particularly beneficial for human health as a natural nutritional supplement.Keywords:Acacia mearnsii;proanthocyanidins;in vitro digestion;antioxidant;antidiabetic;HPLC/MS
研究领域:
食品科学
·
营养学
·
药理学
✓ 已验证
DOI
PubMed
高影响因子
MOLECULES
·
2018
·Vol. 23
·期 11
·2891
·
IF 3.098
Xiao Chen,Jia Xiong,Shenlin Huang,Xun Li,Yu Zhang,Liping Zhang,Fei Wang
The proanthocyanidins from ethanol extracts (80%,v/v) ofAcacia mearnsii(A. mearnsii) bark on chemical-based and cellular antioxidant activity assays as well as carbolytic enzyme inhibitory activities were studied. About 77% of oligomeric proanthocyanidins in ethanol extracts ofA. mearnsiibark were found by using normal-phase HPLC. In addition, HPLC-ESI-TOF/MS and MALDI-TOF/TOF MS analyses indicated that proanthocyanidins fromA. mearnsiibark exhibited with a degree of polymerization ranging from 1 to 11. These results of combined antioxidant activity assays, as well as carbolytic enzyme inhibitory activities of proanthocyanidins fromA. mearnsiibark, indicated an encouraging antioxidant capacity for the high polyphenol content and a potential for use as alternative drugs for lowering the glycemic response.Keywords:proanthocyanidins;HPLC/MS;MALDI-TOF/MS;antidiabetic;antioxidant;degree of polymerization
研究领域:
药理学
·
生物化学
·
分析化学
✓ 已验证
产品关联
DOI
PubMed
高影响因子
FOOD CHEMISTRY
·
2020
·
IF 6.306
Zhenlan Xu,Lingxiangyu Li,Yi Xu,Shanshan Wang,Xiaoxia Zhang,Tao Tang,Jianzhong Yu,Huiyu Zhao,Shenggan Wu,Chunrong Zhang,Xueping Zhao
Dendrobium officinale Kimura et Migo ( D. officinale ) is a dual-use plant with both botanical medicine and food applications, drawing increasing attentions. Pesticides are inevitably applied on D. officinale in commercial artificial-sheltered cultivation, yet little is known about pesticide residue levels in D. officinale . A modified high through-put QuEChERS method coupled with HPLC-MS/MS was developed and validated to detect 76 pesticides in D. officinale . Graphitized multi-wall carbon nanotubes (g-MWCNTs) was selected as the clean-up sorbent, showing relative weak affinity to triazole fungicide having planar structure in their molecular and low matrix effects of pesticides in D. officinale samples compared to MWCNTs and pesticarb. The validated method was applied to analyze pesticide residues in 86 real D. officinale samples collected from three main producing provinces. 43 different pesticides were detected with highest residue of 6.11 mg/kg for dimethomorph. Given possible health risks related to pesticide residues, accordingly, risk assessment of human exposure to pesticides via intake of D. officinale was thus performed, indicating that the pesticide residue in fresh or dry D. officinale would not cause potential risk to human health either in the long-term or short-term. This work improved our understanding of potential exposure risk of pesticide multi-residues in D. officinale .
研究领域:
药用植物学
·
食品科学
·
分析化学
·
毒理学
✓ 已验证
产品关联
DOI
PubMed
高影响因子
JOURNAL OF CHROMATOGRAPHY A
·
2022
·
IF 4.601
Jiating Zheng,Xiaoru Peng,Taifeng Zhu,Shuyao Huang,Chao Chen,Guosheng Chen,Shuqin Liu,Gangfeng Ouyang
In recent years, bile acids (BAs), the important component of bile, were found closely related to the occurrence and development of diseases, therefore, determination of BAs in bile samples is of great significance. However, biological matrix complexity and low concentrations of BAs were still challenging for BA detection in small amount of bile samples. In this work, a core-shell NH 2 -MIL101@mSiO 2 was designed to improve the capture ability of BAs in biological samples, as well as possess good biocompatibility. Subsequently, solid-phase microextraction (SPME) probe of the NH 2 -MIL101@mSiO 2 was coupled with HPLC-MS/MS to establish the analysis method for detecting eight BAs in bile samples. The established method received extraction efficiencies of (30–2143)-fold higher than those of the commercial probes and low limit of detection (LOD ≤ 0.21 ng mL −1 ). The miniaturization of SPME sampling devices, as well as the low LOD of this work, endowed this method advantage of low consumption of bile samples (30 μL). Based on the proposed method, eight BAs in bile samples of pancreatic cancer patients and cholelithiasis patients were detected successfully. A distinct difference was found in the concentrations of four targeted BAs in bile samples from pancreatic cancer patients and cholelithiasis patients. This work provided a method for quantification of eight BAs in small volume human bile samples, and it could open up a perspective regarding the relationship between BA metabolism and the occurrence of diseases.
研究领域:
分析化学
·
生物医学工程
·
临床生化
✓ 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）