Food Analytical Methods
·
2024
·
IF 2.6
Pan Xingyu,Chen Jinzi,Guo Tao,Kuang Fengjiao,Kang Zonghua,Luo Jianguang
Betel nut (Areca nut, AN) products are extensively consumed across East and South Asian countries, with Binglang being the predominant chewable AN product in China. Given the increased risk of carcinogenicity associated with alkaloid nitrogen oxides compared to the primary alkaloids in AN, this study aimed to establish a precise and sensitive method for quantitative analysis of the arecoline N-oxide (ACNO) and arecaidine N-oxide (ADNO) at three different processing stages of Binglang using liquid chromatography-tandem mass spectrometry (LC–MS/MS). The developed method underwent comprehensive validation, evaluating key analytical parameters including selectivity, linearity, sensitivity, accuracy, precision, and stability. Notably, the method demonstrated excellent sensitivity, with the limits of detection (LOD) ranging from 0.029 to 0.135 ng/mL, while the limits of quantification (LOQ) ranging from 0.095 to 0.450 ng/mL. Subsequently, the established analytical technique was applied to analyze 15 Binglang samples at three different processing stages, providing the first evidence of the content and variability of alkaloid nitrogen oxides throughout these stages. ACNO and ADNO were detected in all samples, and their total contents ranged from 4.31 to 32.82 μg/g. The changes observed across different processing stages indicated that the roasting process at 80 ℃ resulted in the promotion of alkaloid nitrogen oxides. This analytical approach constitutes a valuable tool for the quality control and risk assessment of Binglang and can be extended to other AN products, thereby assisting in addressing health concerns associated with these products.
研究领域:
药理学
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分析化学
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食品安全
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DOI
高影响因子
Frontiers in Pharmacology
·
2024
·
IF 4.4
Zhao Huan,Hu Xueli,Guan Shenghong,Cai Jinhong,Li Xiaohan,Fang Jiaxi,Lin Bo,Zhu Wei,Tian Jingkui,Jin Juan,He Qiang,Zhang Xiaoyong
Introduction: Some herbal ingredients can reshape the composition of the gut microbiome as well as its metabolites. At the same time, the gut microbiota can also affect drug metabolism. A large number of studies have reported that saponins are biotransformed under the action of intestinal microorganisms to improve drug efficacy and bioavailability. Capilliposide A is a triterpenoid saponin, which is derived from Lysimachia capillipes Hemsl. CPS-A has anti-inflammatory pharmacological activity, but the substance basis in vivo is unknown at present, so studies on the interaction between intestinal microorganisms and CPS-A may clarify the pharmacodynamic substance basis of CPS-A.Methods: This study established a colitis mouse model, collected sterile feces from normal mice and colitis mice, and incubated CPS-A with two different intestinal flora in vitro. Based on LC-MS, the metabolic process of CPS-A mediated by intestinal microbes and the intervention effect of CPS-A on intestinal microbiome derived metabolites were studied.Results: The results of experiments indicate that intestinal microorganisms can mediate the biotransformation of CPS-A and metabolize it into corresponding deglycosylation products, thereby promoting its drug effect. Not only that, CPS-A can also promote metabolites such as Deoxycholic acid, Histamine, 3-Hydroxytridecanoic acid, and Indole-3-acetic acid in the intestinal microbiota of mice with colitis. This may result in anti-colitis effects. CPS-A mainly involved in metabolic pathways such as azathioprine and mercaptopurine, which may also have beneficial or adverse effects.Discussion: This study on the interaction between CPS-A and microbiota provides a new idea for the study of traditional Chinese medicine with poor oral bioavailability. The regulatory effect of CPS-A on the metabolites of intestinal flora in colitis mice was also found. It laid a foundation for exploring the mechanism of action of saponins on colitis mice.
研究领域:
药理学
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微生物学
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代谢组学
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DOI
PubMed
高影响因子
JOURNAL OF PHARMACEUTICAL AND BIOMEDICAL ANALYSIS
·
2022
·
IF 3.571
Xiaoli Zhang,Na Yang,Min Wang,JiaJia Ge,Huaijun Zhu,Jun He,Weihong Ge
Gestational diabetes mellitus (GDM) is not only a threat to the health of pregnant women, but also has profound effects on the health of offspring. Studies have shown that the imbalance of estrogen metabolism is associated with an increased risk of GDM. In this study, an ultra-performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS) method was established and validated for simultaneous quantification of thirteen estrogens in the urine of GDM women, including estrone (E1), estradiol (E2), estriol (E3), and their hydroxylated and methylated metabolites. The method was achieved on a Waters CORTECS C18 column (2.1 mm × 150 mm, 1.6 µm) within 8.5 min. The linear range of thirteen estrogens in urine was 2–1000 pg·mL −1 . Both intra- and inter-day precision for each analyte were less than 15%, with accuracies ranging from 8.3% to 7.3%. The extraction recoveries rate were between 86% and 111%, and stability verification results met the requirements for determination of biological samples. The results suggested that the concentrations of estrogens in all urine samples range from 0.08 to 134.06 (pg·mg −1 creatinine). The mean levels of E1, E2 and most estrogen metabolites in the urine of GDM women were higher than those in healthy pregnant women. Notably, the mean level of 2-hydroxyestrone (2-OHE1) in GDM women was 13.2-fold lower than that in healthy pregnant women. The types of estrogens with the highest mean levels in the urine of GDM and healthy pregnant women were obviously different, which are 2-methoxyestrone (2MeOE1) and E3, respectively. Our results demonstrated that this specific and sensitive method is suitable for quantifying estrogens in human urine and could provide support for further research on estrogen-related pathological mechanisms in GDM and other diseases.
研究领域:
医学
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内分泌学
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分析化学
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PubMed
高影响因子
JOURNAL OF MASS SPECTROMETRY
·
2026
·Vol. 61
·期 5
·e70057
·
IF 2.1
Daomiao Huang,Hong Chen,Hai Zhang,Xin Dong
In assisted reproductive technology (ART), controlled ovarian hyperstimulation (COS) plays an important role in guiding treatment progress and determining success. Many ovulation-inducing agents are used in this process, including human menopausal gonadotropin (HMG), recombinant follicle-stimulating hormone (r-FSH), recombinant luteinizing hormone (r-hLH), urinary human chorionic gonadotropin (u-hCG), and recombinant human chorionic gonadotropin (r-hCG). HMG, which comes from the urine of postmenopausal women, mainly contains FSH, LH, and hCG. While bioactivity-based potency units and immunoassay-based ELISA methods remain the gold standard for quantifying protein therapeutics, LC–MS/MS is emerging as a game-changing technology. Its unique strengths are exceptional specificity and absolute quantification capabilities, independence from specialized reagents, powerful multiplexing potential, and ability to provide structural insights, establishing it as an essential tool for both orthogonal verification and cutting-edge research in the field. This study used reverse-phase liquid chromatography with mass spectrometry (RP-LC–MS/MS) and a label-free quantitative proteomics method to analyze imported r-hFSH, r-hLH, r-hCG (Gonal-F, Luveris, and Ovidrel), three domestic HMG products (Le Baode, Man Fuxin, and Xin Yunle), and u-hCG (Li Zhu). The results showed that the purity of the main component in imported gonadotropin drugs was higher than 98.55%. On the other hand, the main element of domestic u-HMG is FSH, with small amounts of hCG and very little LH. These results reveal significant differences in the composition of imported and domestic gonadotropin products, underscoring the need to further evaluate their biological activity and clinical effectiveness. This study provides important insights into drug selection for ART, with practical value for improving the quality of HMG drugs and making better use of them in clinical settings.
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高影响因子
JOURNAL OF PHARMACOLOGICAL AND TOXICOLOGICAL METHODS
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2026
·
IF 2.1
Zhenhua Zhang,Bingchen Ge,Yanyu Wang,Changrui Long,Huixing Wu,Hui Chen,Shijian Xiang,Benjie Zhou
Objective To develop a novel approach for quantitative analysis of three pharmaceutical agents commonly employed in the treatment of hematological disorders (venetoclax, busulfan, and voriconazole) by liquid chromatography tandem mass spectrometry (LC-MS/MS). Methods The internal standards were venetoclax-d8 (venetoclax), busulfan-d8 (busulfan), and posaconazole (voriconazole), which were separated on a Phenomenex Kinetex® C 18 (2.1 × 50 mm, 2.6 μm) column, and the multiple reaction monitoring was carried out in the positive ion mode of the SCIEX Triple Quad™ 5500. Protein precipitation pretreatment was performed using acetonitrile, with solvent A (2 mmol/L ammonium acetate dissolved in water containing 0.1% formic acid) and solvent B (acetonitrile solution containing 0.1% formic acid) as mobile phases. The flow rate was 0.8 mL/min, and the injection volume was 5 μL. Results The method was validated with regards to selectivity, lower limit of quantification, linearity, precision and accuracy, matrix effect and extraction recovery, dilution integrity, and stability. The runtime of each plasma sample was 3.1 min. The concentration ranges of the calibration curves were 50–10,000 ng/mL for venetoclax and voriconazole, and 15–3000 ng/mL for busulfan, with all the three correlation coefficients greater than 0.999. There were significant drug–drug interactions with venetocalx and voriconazole, and the incidence of adverse reactions was related to the venetoclax exposure in vivo. Concentrations of busulfan and voriconazole showed substantial interindividual variability. Conclusion This study develops, with validation, a novel LC-MS/MS method for simultaneous determination of venetoclax, busulfan, and voriconazole, which is suitable for application to therapeutic drug monitoring in patients with acute myeloid leukemia.
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高影响因子
Biosensors-Basel
·
2026
·Vol. 16
·期 6
·311
·
IF 6.2
Xiqiong Mu,Yaqin Dong,Ling Jin,Tiantian Zhu
This study compares the performance of novel fluorescent nanobiosensors and liquid chromatography–mass spectrometry (LC-MS) for detecting organophosphorus pesticide residues inAngelica sinensis. Key parameters such as recovery rate and relative standard deviation (RSD) were evaluated to identify a preferable detection method. The results show that the fluorescent nanobiosensor offers superior sensitivity, whereas LC-MS excels in accuracy and quantitative analysis. For phoxim, the GQDs@GSH sensor achieved an LOD of 0.075 μmol·L−1, with recoveries of 97.65–100.62% (RSD < 3.35%). For glyphosate, the PDOA/Cu2+sensor achieved an LOD of 1.8 nmol·L−1, and the AgNCs sensor achieved an LOD of 21 nmol·L−1, with recoveries of 91.30–105.34% (RSD < 3.35%). The originality of this work is threefold and does not claim de novo synthesis of unknown materials: (i) it is the first validation of three existing fluorescent nanosensors (GQDs@GSH, PDOA/Cu2+, and AgNCs) specifically for organophosphorus pesticide detection in the complex medicinal plant matrixAngelica sinensis; (ii) it provides the first systematic comparison of these nanosensors against the pharmacopeia-standard LC-MS method in this matrix, delineating their complementary advantages; (iii) it is the first assessment of their phytotoxicity inAngelica sinensisseedlings, demonstrating biocompatibility and potential for in planta imaging.
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PubMed
高影响因子
ANALYTICAL AND BIOANALYTICAL CHEMISTRY
·
2019
·Vol. 411
·期 15
·3361-3372
·
IF 3.286
Zhang Yingyi,Li Liang,Wang Qi,Shen Mei,Han Weili,Yang Xuemei,Chen Lingyun,Ma Ande,Zhou Zhengzheng
Methamphetamine (METH) is one of the most highly addictive illicit drugs abused all over the world. Much evidence indicates that METH abuse leads to major toxicity, medical consequences, and even severe public health consequences. Existing studies usually focus on the pathomechanism of METH-induced toxicity; therefore, data on metabolites and elements correlating with particular toxicity remain scarce. The objective of the present study is to develop appropriate analytical procedures to identify the differential metabolic and elemental biomarkers on METH-induced hepatic injury to rats. The rats were administrated with METH (15 mg/mL/kg, two times per day) via intraperitoneal (i.p.) injections for four consecutive days. The alanine aminotransferase and aspartate aminotransferase activity levels of in the rat serum of the METH group increase significantly compared with those of the control group, suggesting obvious hepatic injury. The results are further confirmed by the histopathological microscopic observation. A total of 18 small molecular metabolites and 19 elements are selected to perform the simultaneous quantification based on the combination of liquid chromatography coupled with tandem mass spectrometry and inductively coupled plasma mass spectrometry. Sample preparation was optimized to cover all the analytes. Both methods are optimized and validated according to developed guidelines such as limits of detection, limits of quantification, linearity, precision, and recovery. All the obtained data are within the satisfactory range. The normalized data were processed according to the partial least squares discrimination analysis (PLS-DA) model. Five differential metabolic and six elemental markers are identified in rat plasma based on the variable importance in projection (VIP) (> 1) and t test results. Overall, the results obtained in this study demonstrate the developed methods are suitable for simultaneous determination of metabolic and elemental markers in the hepatic injury to rats induced by METH.
Graphical abstract
研究领域:
毒理学
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分析化学
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药理学
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病理学
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DOI
PubMed
高影响因子
JOURNAL OF PHARMACEUTICAL AND BIOMEDICAL ANALYSIS
·
2019
·
IF 2.983
Shuai Ji,Xian Shao,Zhen-yu Su,Lei Ji,Yu-jie Wang,Yun-su Ma,Lu Zhao,Yan Du,Meng-zhe Guo,Dao-quan Tang
Fufang Danshen Dripping Pill (FDDP) and Clopidogrel Bisulfate Tablet (CBT) are usually combined for treatment of coronary artery diseases in clinical. To investigate the pharmacokinetic interaction between FDDP and CBT after oral administration of FDDP, CBT and their combination in rats, a novel LC–MS method with segmented scan modes (multiple reaction monitoring and selected ion monitoring) and polarity (positive and negative ionization) was developed. Clopidogrel and the main active ingredients of FDDP, with different chemical and ionization properties, were simultaneously quantified in plasma in a single run. The method was validated in terms of specificity, linearity, precision, accuracy, recovery, matrix effect and stability. As a result, co-administration of FDDP and CBT significantly altered the pharmacokinetic parameters of danshensu, ginsenoside Rb1, dihydrotanshinone I, tanshinone I and tanshinone IIA of FDDP, as well as clopidogrel. Mechanism studies suggested that induction of liver cytochrome P450 isozymes CYP2C11 and CYP3A1 by co-administration, as well as inhibition of carboxyl esterase 1, was partly responsible for FDDP-CBT pharmacokinetic interactions. The developed LC–MS method could be used to simultaneously quantify different types of in vivo analytes in a single run, and the results could be used for clinical medication guidance of FDDP and CBT.
研究领域:
药理学
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分析化学
·
药学
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PubMed
高影响因子
MOLECULES
·
2023
·Vol. 28
·期 22
·7634
·
IF 4.6
Hongbo Yang,Jin Li,Jianfei Mao,Chan Xu,Jieyu Song,Feng Xie
Ochratoxins, a common class of mycotoxin in capsicum, and techniques and methods for the determination of mycotoxins in spices have been increasingly developed in recent years. An innovative and eco-friendly method of dispersive liquid–liquid microextraction (DLLME) was demonstrated in this study, based on a synthesized deep eutectic solvent (DES) combined with LC-MS/MS, for the quantification and analysis of two ochratoxins in capsicum. The DES-DLLME method parameters entail selecting the DES type (thymol:decanoic acid, molar ratio 1:1) and DES volume (100 μL). The volume of water (3 mL) and salt concentration (0 g) undergo optimization following a step-by-step approach to achieve optimal target substance extraction efficiency. The matrix effect associated with the direct detection of the target substance in capsicum was significantly reduced in this study by the addition of isotopic internal standards corresponding to the target substance. This facilitated optimal conditions wherein quantitative analysis using LC-MS/MS revealed a linear range of 0.50–250.00 µg/mL, with all two curves calibrated with internal standards showing correlation coefficients (r2) greater than 0.9995. The method’s limits of detection (LODs) and limits of quantification (LOQs) fell in the ranges of 0.14–0.45 μg/kg and 0.45–1.45 μg/kg, respectively. The method’s spiked recoveries ranged from 81.97 to 105.17%, indicating its sensitivity and accuracy. The environmental friendliness of the technique was assessed using two green assessment tools, AGREE and complexGAPI, and the results showed that the technique was more in line with the concept of sustainable development compared to other techniques for detecting ochratoxins in capsicum. Overall, this study provides a new approach for the determination of mycotoxins in a complex food matrix such as capsicum and other spices using DES and also contributes to the application of green analytical chemistry methods in the food industry.Keywords:deep eutectic solvent;dispersive liquid–liquid microextraction;ochratoxins;capsicum;green analytical chemistry
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Analytical Methods
·
2014
·Vol. 6
·期 21
·8675-8681
·
IF 1.938
Waner Hou,Guanghui Liu,Xiuman Sun,Zhiyong Xie,Rongbiao Pi,Wei He,Manna Lin,Qiongfeng Liao
The aim of the present work was to develop and validate an LC-MS/MS method with electrospray ionization (ESI) for the quantification of lipoic acid–fasudil dimer (L–F 001), a novel multi-functional neuroprotective drug in rat plasma, using tetrahydropalmatine as an internal standard. The separation was carried out on a C18 column using a mobile phase consisting of acetonitrile and water (containing 5 mmol l−1 ammonium acetate adjusted to pH 5.0 with formic acid). The detection was performed by multiple reactions monitoring (MRM) mode via ESI source operating in the positive ionization mode. An linear calibration curve was obtained over the concentration range of 1.0–1000.0 ng ml−1 for lipoic acid–fasudil dimer (L–F 001). Accuracy, precision and extraction recovery of the analyte was satisfactory. The validated method was successfully applied to monitor the pharmacokinetic profile of the lipoic acid–fasudil dimer (L–F 001) after oral administration to rats.
研究领域:
药物分析
·
神经科学
·
药理学
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DOI
高影响因子
ANALYTICAL AND BIOANALYTICAL CHEMISTRY
·
2018
·Vol. 410
·期 7
·2011-2018
·
IF 3.307
Yu Lingling,Wen Chao,Li Xing,Fang Shiqi,Yang Lichuan,Wang Tony,Hu Kaifeng
Quantification of endogenous and exogenous plasma glucose can help more comprehensively evaluate the glucose metabolic status. A ratio-based approach using isotope dilution liquid chromatography tandem mass spectrometry (ID LC-MS/MS) with indirect multiple reaction monitoring (MRM) of the derivative tag was developed to simultaneously quantify endo-/exogenous plasma glucose. Using diluted D-[ 13 C 6 ] glucose as tracer of exogenous glucose, 12 C 6 / 13 C 6 glucoses were first derivatized and then data were acquired in MRM mode. The metabolism of exogenous glucose can be tracked and the concentration ratio of endo/exo-genous glucose can be measured by calculating the endo-/exo-genous glucose concentrations from peak area ratio of specific daughter ions. Joint application of selective derivatization and MRM analysis not only improves the sensitivity but also minimizes the interference from the background of plasma, which warrants the accuracy and reproducibility. Good agreement between the theoretical and calculated concentration ratios was obtained with a linear correlation coefficient ( R ) of 0.9969 in the range of D-glucose from 0.5 to 20.0 mM, which covers the healthy and diabetic physiological scenarios. Satisfactory reproducibility was obtained by evaluation of the intra- and inter-day precisions with relative standard deviations (RSDs) less than 5.16%, and relative recoveries of 85.96 to 95.92% were obtained at low, medium, and high concentration, respectively. The method was successfully applied to simultaneous determination of the endo-/exogenous glucose concentration in plasma of non-diabetic and type II diabetic cynomolgus monkeys.
Graphical Abstract The scheme of the proposed ratio-based approach using isotope dilution LC-MS/MS with indirect MRM of the derivative tag for simultaneous quantification of endogenous and exogenous plasma glucose.
研究领域:
分析化学
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代谢组学
·
生物医学科学
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DOI
PubMed
高影响因子
ANNALS OF MEDICINE
·
2023
·
IF 4.4
Zhengwen Xu,Youran Li,Ying Liu,Shengmin Liu,Lin Zhang,Jing Wang,Shaofei Su,Lin Liu,Lanlan Meng,Hongyuan Zhu,Jingru Sun,Lijun Shao,Lin Li,Yanhong Zhai,Guanghui Li,Zheng Cao
Background As folates are essential for embryonic development and growth, it is necessary to accurately determine the levels of folates in plasma and red blood cells (RBCs) for clinical intervention. The aims of this study were to develop and validate a liquid chromatography-tandem mass spectrometry (LC-MS/MS) method for quantitation of folates in plasma and RBCs and to examine the association between plasma and RBC folate concentrations and gestational diabetes mellitus (GDM), gestational hypertension (GH) and preeclampsia (PE).Methods With the in-house developed LC-MS/MS, a retrospective cross-sectional study was conducted. The healthy pregnant women of first- (n = 147), second- (n = 84) and third-trimester (n = 141) or the women diagnosed with GDM (n = 84), GH (n = 58) or PE (n = 23), that were aged between 22 and 46 years old and registered at our institute, were subjected for measurement of folic acid (FA) and 5-methyltetrahydrofolate (5-MTHF), followed by appropriate statistical association analysis.Results The assay for simultaneous quantitation of FA and 5-MTHF in plasma and RBCs was linear, stable, with imprecision less than 15% and recoveries within ±10%. The lower limits of quantification for FA and 5-MTHF measurement in whole blood were 0.57 and 1.09 nmol/L, and in plasma were 0.5 and 1 nmol/L, respectively. In the association analysis, the patients with lower RBC folate level (<906 nmol/L) presented higher risks of PE development (OR 4.861 [95% CI 1.411–16.505]) by logistic regression and restricted cubic spline (RCS) regression in a nonlinear fashion. In addition, higher level of plasma folates in pregnancy was significantly associated with GH risk but may be protective for the development of GDM.Conclusions The in-house developed LC-MS/MS method for folates and metabolites in plasma or RBC showed satisfactory analytical performance for clinical application. Further, the levels of folates and metabolites were diversely associated with GDM, GH and PE development.
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高影响因子
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