JOURNAL OF PHARMACEUTICAL AND BIOMEDICAL ANALYSIS
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2023
·
IF 3.4
Fenglun Zhao,Zheng Xiang,Junping Han,Jie Pan,Yuchen Qu,Kai Fan,Zhiqiang Wu,Delai Xu,Yunli Yu,Zhu Shen,Cunjin Su
In December 2021, the U.S. Food and Drug Administration (FDA) granted emergency authorization for Paxlovid® as an antiviral treatment for COVID-19. Paxlovid® is composed of two tablets, nirmatrelvir and ritonavir. Dose adjustment is necessary in cases of renal insufficiency. The aim of present study is to establish a LC–HRMS method for simultaneous determination of nirmatrelvir/ritonavir in human serum for therapeutic drug monitoring. Internal standard saquinavir was added in 25 μL human serum samples, and then the samples were precipitated with methanol. The analytes were separated by gradient elution on a C18 column, using a mobile phase of 0.1 % formic acid-water and methanol, at a flow rate of 0.4 mL/min. The injection volume was 2 μL, and the analysis time was 5 min. The determination of the analytes was performed by electrospray ionization in positive mode by full mass monitoring. The detected ions of nirmatrelvir, ritonavir and saquinavir were m/z 500.24792, 721.32004 and 671.39155, respectively. The linear concentration range for nirmatrelvir was 78.13–20000 ng mL −1 , for ritonavir was 15.63–4000 ng mL −1 (r 2 ＞0.9900). The accuracy ranged from 87.45 %∼104.63 %, and the intra-day and inter-day precision RSD was <15 %. The recovery of nirmatrelvir ranged from 98.72 %∼109.83 %, and that of ritonavir was 95.41∼112.36 %. The matrix effect of nirmatrelvir was 88.31∼97.73 %, and that of ritonavir was 85.17∼103.05 %. This method was used to measure the trough concentrations of nirmatrelvir/ritonavir in 17 patients. The trough concentration of nirmatrelvir was 1331.7–8352.5 ng/mL, and that of ritonavir was 53.4–1325.5 ng mL −1 , with large individual differences. The method is simple, sensitive, specific, and reproducible, and can be used for monitoring the blood concentration and pharmacokinetic study of nirmatrelvir/ritonavir in COVID-19 patients.
研究领域:
药理学
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分析化学
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临床医学
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DOI
PubMed
高影响因子
FOOD CHEMISTRY
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2020
·
IF 6.306
Chaonan Su,Caihong Li,Kang Sun,Wenjing Li,Rongxia Liu
Walnut leaves are rich in phenolic components with antibiotic and antioxidative effects. However, few studies have reported the quantitative analysis of active components in walnut leaf. In this study, a novel method for quantifying the active components in walnut leaves was developed by combining ultra-high performance liquid chromatography-hybrid quadrupole-Orbitrap high-resolution mass spectrometry (UHPLC-Q-Orbitrap HRMS) with quantitative analysis of multi-components by a single marker (QAMS). In total, 13 bioactive components were analyzed by a single marker, quercetin. To evaluate the accuracy of this method, an auxiliary quantification method with 13 reference standards was established and validated. The standard method differences (SMDs) of the quantification results between QAMS and the auxiliary method were lower than 20%, indicating that the QAMS method can accurately determine the active components in walnut leaves. This method can provide a reference to address the absence of reference standards for analyzing other foods and herbs.
研究领域:
植物化学
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分析化学
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药学
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DOI
PubMed
高影响因子
BIOMEDICAL CHROMATOGRAPHY
·
2020
·Vol. 34
·期 9
·e4870
·
IF 1.728
Jiping Yi,Bin Chen,Yongzheng Bao,Jingyu Wang
In this study, a simple and reliable LC–MS/MS method was first proposed for the simultaneous determination of TUG-891 and its metabolites TUG-891-alcohol, TUG-891-aldehyde, and TUG-891-acid in rat plasma. The analytes and fasiglifam (internal standard) were extracted from plasma samples with acetonitrile and separated using an Acquity BEH C 18 column (1.7 μm, 2.1 × 50 mm) with water containing 0.05% ammonium hydroxide and acetonitrile containing 0.05% ammonium hydroxide as the mobile phase. A Q-Exactive Orbitrap mass spectrometer in full-scan mode was used for mass detection, and the data analysis was obtained using a mass extraction window of 5 ppm. The calibration curves exhibited excellent linearity (correlation coefficient > 0.9981) in the concentration range of 0.5–1000 ng/mL. The lower limit of quantification was 0.5 ng/mL for all analytes. The intra- and inter-day precision was less than 11.31%, and the accuracy ranged from −11.50 to 9.50%. The extraction recovery of the analytes from rat plasma was greater than 82.31%, and no obvious matrix effect was found. The established method was further applied to the pharmacokinetic study of TUG-891, TUG-891-alcohol, TUG-891-aldehyde, and TUG-891-acid in rat after a single dose of 5-mg/kg treatment of TUG-891. The results demonstrated that TUG-891 was rapidly metabolized into its metabolites and the systemic exposures of the metabolites were much higher than those of TUG-891.
研究领域:
分析化学
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药物代谢
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药理学
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DOI
PubMed
高影响因子
Chemosensors
·
2023
·Vol. 11
·期 3
·165
·
IF 4.2
Yi Lv,Feng-Lian Ma,Jia-Nan Wang,Yao Zhang,Yuan Jiang,Qian Ge,Yong-Jie Yu
The time involved and the high economic cost of using oak barrels to age wines have led to a significant price difference compared to non-oak barrel aged wines and may lead to some fraudulent sales in the market. In this study, an untargeted metabolomic strategy was developed to detect the metabolite composition of oak barrel aged and non-oak barrel aged wines in both positive and negative ion modes by using UHPLC–HRMS combined with the recently developed chemometric method AntDAS. The results of partial least squares discrimination analysis (PLS-DA) showed that the samples were characterized into two categories. Finally, 51 compounds were identified in positive ion mode, while 26 compounds were identified in negative ion mode. The results indicate that combining UHPLC–HRMS with AntDAS can reveal the material basis of wines and has excellent potential to differentiate between oak barrel aged and non-oak barrel aged wines.Keywords:oak barrel aged wines;UHPLC-HRMS;AntDAS;chemometrics
研究领域:
食品科学
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分析化学
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化学计量学
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DOI
高影响因子
JOURNAL OF HAZARDOUS MATERIALS
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2022
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IF 14.224
Xiao Wang,Ya Zhao,Xin Qi,Tiantian Zhao,Xiupin Wang,Fei Ma,Liangxiao Zhang,Qi Zhang,Peiwu Li
Aflatoxins seriously threaten human health and food safety, and early warning benefits the reasonable use of control measures to reduce aflatoxin contamination. In this study, a novel method for quantifying aflatoxins and their precursors in the aflatoxin biosynthesis pathway was developed by combining ultra-high performance liquid chromatography high-resolution mass spectrometry (UHPLC-HRMS) with quantitative analysis of multi-components by a single marker (QAMS). The stability of the relative correction factor (RCF) of QAMS was then systematically evaluated. The validation results showed that the relative deviation (RD) between QAMS and the external standard method (ESM) was less than 11.7%, indicating that the established QAMS method could replace ESM without the use of reference standards. This method was successfully employed to compare the time-course changes of metabolites in the aflatoxin biosynthesis pathway of Aspergillus flavus and Aspergillus parasitica. As a result, the precursors of (1'S,5′R)−5′-Hydroxyaverantin (HAVN) and Versicolorin B (VerB) could be used as potential markers for the early warning of aflatoxin contamination. This study provided a quantitative method of aflatoxins and their precursors in the biosynthesis pathway, and may serve as a reference for the extension of quantitative studies on other metabolic pathways.
研究领域:
食品安全
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分子生物学
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DOI
PubMed
高影响因子
Journal of Food Measurement and Characterization
·
2024
·
IF 2.9
Wang Jin,Ren Qiao,Zhou Houqin,He Chenghao,Huang Qinwan
Red ginseng, a processed product of ginseng, has been shown to possess various pharmacological effects. To investigate the changes in ginsenosides during the processing of ginseng into red ginseng and to visualize their spatial distribution characteristics in tissues, ultra-high performance liquid chromatography coupled with hybrid quadrupole-orbitrap high-resolution mass spectrometry (UPLC-Q-Orbitrap HRMS) was used to detect and identify the extracts of ginseng and red ginseng. Matrix-assisted laser desorption/ionization mass spectrometry imaging (MALDI-MSI) was used to visually analyze the spatial distribution and temporal changes of prototype ginsenosides and their metabolites in ginseng. The UPLC-Q-Orbitrap HRMS results showed the identification of 42 major ginsenosides in both ginseng and red ginseng. Additionally, PCA and OPLS-DA analyses identified the processing-related markers for ginseng and red ginseng. During the processing of ginseng into red ginseng, the content of protopanaxadiol ginsenosides decreased (Rb1, Rc, Rd, etc.), while the types and content of rare ginsenosides increased (Rg3, Rg5, Rh1, etc.). The MALDI-MSI tissue distribution results demonstrated that ginsenosides in ginseng were mainly distributed in the cambium and phloem, while the processing led to the transformation of ginsenosides and an increase in distribution in the xylem and medulla. This study comprehensively reveals the chemical diversity and dynamic transformation patterns during the processing of ginseng, providing more substantial foundational information for research on red ginseng processing techniques. The transformation of these rare ginsenosides also indicates that ginseng is more beneficial for pharmacological applications such as anti-tumor, anti-allergic, and liver protection after being processed into red ginseng. Graphical abstract
研究领域:
药用植物学
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分析化学
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中药学
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产品关联
DOI
高影响因子
INDUSTRIAL CROPS AND PRODUCTS
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2021
·
IF 5.645
Caihong Li,Yan Zhao,Wenjing Li,Rongrong Xing,Jing Lu,Rongxia Liu
Euodiae Fructus (EF, the fruit of Tetradium ruticarpum ) belongs to the family Rutaceae which has a complex genetic background, making classification a challenge. In order to classify the three closely related cultivars (small flower EF, medium flower EF, and big flower EF) and simplify the identification procedure in the future, an approach integrating ultra-high performance liquid chromatography-ultraviolet spectrum-hybrid quadrupole-Orbitrap high resolution mass spectrometry (UHPLC-UV-Q-Orbitrap HRMS) with machine learning algorithms was developed. Orthogonal partial least squares-discriminant analysis (OPLS-DA) and random forest (RF) were used to assort the processed EF products and select the chemical markers to differentiate among the three EF cultivars, respectively. Then the thresholds of classification were determined using the eXtreme Gradient Boosting (XGboost) model based on the quantitative data of chemical markers by the UHPLC-Q-Orbitrap HRMS. The results demonstrated that the approach successfully discriminated among three closely related cultivars of EF, and five chemical markers (neochlorogenic acid, (+)-catechin, chlorogenic acid, dehydroevodiamine, and limonin) were selected. Thresholds were obtained to classify the three cultivars. If the content of neochlorogenic acid was greater than 7.52 mg/g, the sample belonged to small flower EF, otherwise, it belonged to medium flower EF or big flower EF. Furthermore, if the content of dehydroevodiamine was greater than 3.84 mg/g, the sample was medium flower EF, otherwise, it was big flower EF. In general, this research provides a novel strategy for the discrimination of Euodiae Fructus cultivars to avoid misapplication and possible side effects.
研究领域:
药学
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分析化学
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植物学
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产品关联
DOI
高影响因子
CHROMATOGRAPHIA
·
2022
·Vol. 85
·期 12
·1017-1028
·
IF 2.213
Gao Yanlin,Chen Cen,Wang Ren,Li Zehua,Cheng Qiaoyuan
Currently, illegal addition of anti-infective drugs has been detected in some cosmetics to achieve rapid sterilization and anti-inflammatory effects. However, the abuse of anti-infective drugs may endanger the health of citizens. Thus, methods for the detection and quantitative determinations of such substances should be developed. In this paper, a method combining ultra-high-performance liquid chromatography with quadrupole time-of-flight mass spectrometry (UHPLC-Q-TOF HRMS) was designed. Its significance and potential were verified by the identification, confirmation, and quantification of 37 illegally added anti-infective drugs in cosmetics that claimed to have anti-acne effects. The method validation revealed a satisfactory linear relationship, and each coefficient of determination ( r 2 ) was higher than 0.9943. The LOD and LLOQ results were in the ranges of 0.0003–0.1063 μg g −1 and 0.0012–0.3545 μg g −1 , respectively. The accuracy ranged from 70.8 to 122.8%, whereas the intra- and inter-day precisions were in the ranges of 0.2–12.8% and 0.2–13.8%, correspondingly. The mean recoveries were in the range of 70.1–117.7%, and the matrix effects ranged from 73.0 to 121.4%. Of the 200 batches of cosmetics that claimed to have anti-acne effects, three batches were positive, with chemical components such as metronidazole, lincomycin, clindamycin, tinidazole and miconazole nitrate being discovered. Therefore, the Q-TOF spectrometry could be widely applied in routine screening of adulteration in cosmetics.
研究领域:
分析化学
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药学
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医学
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产品关联
DOI
高影响因子
JOURNAL OF ETHNOPHARMACOLOGY
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2020
·
IF 3.69
Rongxia Liu,Chaonan Su,Yumeng Xu,Kangle Shang,Kang Sun,Caihong Li,Jing Lu
Ethnopharmacological relevance Walnut leaf (WL) is a hypoglycemic herbal medication with blood glucose-lowering activity that can affect diabetes mellitus (DM). However, the active components of WL and the mechanisms by which these compounds affect DM are unclear. Aim of study This study aimed to determine these effective ingredients and elucidate the potential mechanisms by which they affect DM via ultra-high performance liquid chromatography-hybrid quadrupole-Orbitrap high-resolution mass spectrometry (UHPLC-Q-Orbitrap HRMS) coupled with network pharmacology analysis. Materials and methods First, UHPLC-Q-Orbitrap HRMS was utilized to identify components of WL. Second, the putative targets of the components were identified and predicted based on chemical similarity and online databases. Third, the key candidate targets and potential active components were identified through topological analysis of a component-disease target interaction network. Finally, interactions between active components and therapeutic targets were confirmed by molecular docking analysis. Results One hundred and thirty components were identified in WL, among which 38 were considered potentially bioactive, as they showed hypoglycemic effects. Among these 38, 8 key active components possessed high similarities and shared 4 targets with approved drugs. These findings were confirmed by molecular docking analysis. Conclusion The approach combining UHPLC-Q-Orbitrap HRMS with network pharmacology analysis is a rapid and effective tool to identify potentially bioactive constituents in medicinal plants and prescriptions.
研究领域:
中药学
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代谢组学
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生物信息学
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产品关联
DOI
PubMed
高影响因子
FOOD CONTROL
·
2022
·
IF 6.652
Zhiyong Zhao,Hengchao E,Enjing Tian,Tingting Fan,Xianli Yang,Xiaobei Li,Yanmei Zhang,Xujiao Li,Ailiang Chen,Changyan Zhou,Xiaoyan Zhao
Foodborne poisoning caused by the cyclopeptide toxins-producing mushroom species seriously endangers human life health. In recent years discovery of new cyclopeptides is getting more attention not only for their toxicity but also for their specific bioactivity. In this study, a combined strategy using liquid chromatography tandem high resolution mass spectrometry and the feature-based molecular networking analysis was established to identify the known cyclopeptide toxins and discover new cyclopeptides in the cyclopeptide toxins-producing mushroom species. The specific fragmentation behaviors of the known cyclopeptide toxins were systematically annotated. Four new phallotoxin analogues were identified for the first time, the chemical structures of which were completely deduced. Moreover, the chemical profiles of the toxic cyclopeptides in lethal mushroom Amanita and Lepiota species were investigated by the self-built cyclopeptides database. The developed strategy could be utilized as a useful tool for identifying the cyclopeptide toxins-induced food poisoning , as well as aid in the discovery of more unknown cyclopeptides.
研究领域:
食品科学
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毒理学
·
分析化学
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产品关联
DOI
高影响因子
Foods
·
2021
·Vol. 11
·期 1
·93
·
IF 4.35
Chenling Qu,Zhuozhen Li,Xiupin Wang
Aspergillus flavusis a common contaminant in grain, oil and their products. Its metabolite aflatoxin B1(AFB1) has been proved to be highly carcinogenic. Therefore, it is of great importance to find possible antifungal substances to inhibit the growth and toxin production ofAspergillus flavus. Carvacrol (CV) was reported as a potent antifungal monoterpene derived from plants. In this paper, the antifungal effects and mechanism of CV onAspergillus flavuswere investigated. CV was shown good inhibition on the growth ofAspergillus flavusand the production of AFB1. CV used in concentrations ranging from 0, 50, 100 and 200 μg/mL inhibited the germination of spores, mycelia growth and AFB1production dose-dependently. To explore the antifungal mechanism of CV onAspergillus flavus, we also detected the ergosterol content ofAspergillus flavusmycelia, employed Scanning Electron Microscopy (SEM) to observe mycelia morphology and utilized Ultra-High-Performance Liquid Chromatography-High-Resolution Mass Spectrometry (UHPLC-HRMS) to explore the lipidome profiles ofAspergillus flavus. The results showed that the production of ergosterol of mycelia was reduced as the CV treatment concentration increased. SEM photographs demonstrated a rough surface and a reduction in the thickness of hyphae inAspergillus flavustreated with CV (200 µg/mL). In positive ion mode, 21 lipids ofAspergillus flavusmycelium were downregulated, and 11 lipids were upregulated after treatment with 200-µg/mL CV. In negative ion mode, nine lipids ofAspergillus flavusmycelium were downregulated, and seven lipids upregulated after treatment with 200-µg/mL CV. In addition, the analysis of different lipid metabolic pathways between the control and 200-µg/mL CV-treated groups demonstrated that glycerophospholipid metabolism was the most enriched pathway related to CV treatment.Keywords:Aspergillus flavus;carvacrol;untargeted lipidomics;ultra-high-performance liquid chromatography-high-resolution mass spectrometry (UHPLC-HRMS);antifungal activity
研究领域:
微生物学
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药理学
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分析化学
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产品关联
DOI
PubMed
高影响因子
Journal of Food Measurement and Characterization
·
2025
·
IF 3.3
Zhong Shu-Rui,Li Yun,Lai Yu-Ping,Luo Er-Lun,Wang Jie,Chen Jing,Du Ye-Gang
Non-targeted metabolomics was employed to analyze metabolites in wet rice noodles fermented by Burkholderia gladioli pv. cocovenenans (BGC) to explore the potential formation of bongkrekic acid (BA). Three groups were incubated for 72 h: the pathogenic strain BGC 83756-inoculated group, the non-pathogenic strain Burkholderia gladioli (BG) 10574-inoculated group, and a blank control (BK) group. Metabolite dynamics were monitored using ultra-performance liquid chromatography-high resolution tandem mass spectrometry (UPLC-HRMS/MS). BA was not detected in either the BK group or the BG 10574-fermented group during incubation. In contrast, BA was first detected in the BGC 83756-inoculated group at 16 h of fermentation and reached a concentration of approximately 4,800 μg/kg in the late stages of culture. A total of 723 and 606 metabolites were identified in negative and positive ion modes, respectively. Differential metabolites, including BA, α-dimorphecolic acid, and calystegine B 5 , were significantly upregulated in the BGC 83756-fermented group compared to the BG 10574-fermented group. Conversely, sinapic acid, saccharopine, 2-methylbutyrylglycine, and 2-keto-6-acetamidocaproate were significantly downregulated. The non-targeted metabolomics analysis of the BA biosynthetic pathway generally aligned with the bon gene cluster predictions, except for β-branching events.
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产品关联
DOI
高影响因子
危险品化学品经营许可证（带存储）