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JOURNAL OF PHARMACEUTICAL AND BIOMEDICAL ANALYSIS · 2022 · IF 3.571

Determination of CYP450 activities in diabetes mellitus rats by a UHPLC-MS/MS method

Zhe Wang,Qing-qing Li,Cheng-ke Huang,Yan-yan Dong,Li-ping Lang,Wei Sun,Jian-chang Qian,Xiao-dan Zhang

In this study, we investigated the effect of type 1 diabetes mellitus on the modulation of the activities of CYP450s in dynamics by a UHPLC-MS/MS method. The diabetic rat model was constructed by an intraperitoneal single injection of streptozotocin . Fasting blood glucose levels > 16.7 mmol/L were considered as diabetic. The rats were given a cocktail of four probe drugs (10 mg/kg phenacetin , 1 mg/kg tolbutamide , 10 mg/kg metoprolol , and 10 mg/kg midazolam) by oral administration for the pharmacokinetic study. Thereafter, the metabolic ratio (MR) of the metabolites to probe substrates were determined. The results indicated that two weeks after diabetes was induced, diabetes increased the MRs of acetaminophen/phenacetin (CYP1A2) and 4-hydroxyl tolbutamide/tolbutamide (CYP2C9); however, it decreased the MRs of α-hydroxy metoprolol/metoprolol (CYP2D6) and 1-hydroxy midazolam/midazolam (CYP3A4). Two months after diabetes was induced, diabetes increased the MRs of acetaminophen/phenacetin and 4-hydroxyl tolbutamide/tolbutamide. The MR of α-hydroxy metoprolol/metoprolol was decreased and the MR of 1-hydroxy midazolam/midazolam was increased but the difference was not significant. According to the results, CYP1A2 and CYP2C9 activities were enhanced in the diabetic rats. and CYP2D6 activity was inhibited in a short period of diabetes; however, the decrease in CYP2D6 activity was not significant in the long period. CYP3A4 activity was decreased in a short period of diabetes and increased in a long period of diabetes but was not significant in the two periods. This study suggests the activity change rule of the CYP450 enzyme system in diabetes mellitus, which can provide a reference for precise clinical medication.

CAS / MDL: 103-90-2 51384-51-1
研究领域: 药理学 · 代谢组学 · 临床医学
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Water · 2024 ·Vol. 16 ·期 9 ·1315 · IF 3

Direct-Injection UHPLC-MS/MS Method for Simultaneous Determination of 78 Illegal Drugs and Psychoactive Substances in Domestic Wastewater

Kan Li,Yiling Hu,Yuke Jiang,Xing Han,Xin Liu,Mingluo Du

The determination of illegal drugs and psychoactive substances in wastewater is increasingly being used to monitor the use of both by populations in specific areas. This article describes a method for the simultaneous determination of 78 illegal drugs and psychoactive substances in wastewater using direct-injection ultra-high-performance liquid chromatography–tandem mass spectrometry (UHPLC-MS/MS). This method includes the analysis of stimulants, opioids, antidepressants, antipsychotic drugs, anti-anxiety drugs, and hallucinogens. The method was validated in terms of the selectivity, calibration range, recovery, matrix effects, accuracy, precision, limit of detection (LOD), and limit of quantification (LOQ). The correlation coefficients were higher than 0.99 for all analytes, and the calibration range was from 0.2 to 500 ng/L. The LOD and LOQ of this method were 0.1–1 ng/L and 0.2–5 ng/L, respectively. The intra- and inter-day precisions were <9.3% and 11.4%, respectively, and the recovery ranged from 81.3% to 117.7%. The method was applied to real domestic wastewater collected from wastewater treatment plants, and the results showed that morphine, codeine, and ephedrine were detected in all samples. Some samples also contained other illegal drugs and psychoactive substances (such as etomidate, methamphetamine, ketamine, and tramadol). This indicates that the direct-injection UHPLC-MS/MS method can be used for the rapid determination of illegal drugs and psychoactive substances in wastewater.

CAS / MDL: 64-18-6
研究领域: 环境科学 · 分析化学 · 毒理学
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FOOD CHEMISTRY · 2022 · IF 9.231

Comparison of two commercial methods with a UHPLC–MS/MS method for the determination of multiple mycotoxins in cereals

Ying-yue Zhang,Mei-juan Zhao,Chun-yao Liu,Kai Ma,Tian-yu Liu,Fei Chen,Li-na Wu,De-jun Hu,Guang-ping Lv

Immunoassay-based techniques are important on-site screening tools for the detection of mycotoxins in cereals. This study aims to evaluate the trueness, precision, repeatability and cross-reactivity of commercially available test strips, ELISA kits and UHPLC-MS/MS on analyzing zearalenone, ochratoxin A, deoxynivalenol, T-2 toxin and fumonisin B 1 . The results showed that false negative rate (25.7 %–37.4 %) of all tested mycotoxins by test strips was higher than the false positive rate (0 %–31.0 %). The repeatability of ELISA kits at the declared LOD dispersed from −85.7 % to +98.4 %. ELISA kits were more accurate at 50 % of the maximum residue limit (MRL) of mycotoxins than 150 % and 200 %. All the tested deoxynivalenol/zearalenone derivatives had cross-reactivity with different level, and sample matrix could reinforce this overestimation of target mycotoxin. This study emphasized that higher-quality antibody screening and more analytical performance investigations are need to address for on-site detection of mycotoxins in the future.

CAS / MDL: 631-61-8 64-18-6
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
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JOURNAL OF CHROMATOGRAPHY B-ANALYTICAL TECHNOLOGIES IN THE BIOMEDICAL AND LIFE SCIENCES · 2016 · IF 2.687

Development and validation of a sensitive UHPLC–MS/MS method for quantitation of prucalopride in rat plasma and its application to pharmacokinetics study

Zhi Sun,Lihua Zuo,Jian Kang,Lin Zhou,Mengmeng Jia,Zeyun Li,Zhiheng Yang,Xiaojian Zhang,Zhenfeng Zhu

A rapid, sensitive, selective and accurate ultra high performance liquid chromatography with tandem mass spectrometry (UHPLC–MS/MS) method was developed and validated for the quantitation of prucalopride in rat plasma using carbamazepine as an internal standard (IS). Separation was achieved on a Waters ACQUITY UHPLC ® HSS C 18 column (2.1   mm   ×   50   mm, 1.8   μm) column with a gradient mobile phase consisting of acetonitrile–water (containing 0.1% formic acid) as mobile phase at a flow rate of 0.2   mL/min. Prucalopride and IS were monitored using positive electrospray triple quadrupole mass spectrometer (Waters Xevo TQD) via multiple reaction monitoring (MRM) mode. The monitored transitions were set at m / z 367.99   →   195.89 and m / z 236.97   →   194.04 for prucalopride and IS, respectively. The achieved lower limit of quantitation was 0.1   ng/mL. The validated method had an excellent linearity in the range of 0.1–100   ng/mL (r   >   0.996). The intra- and inter-day precisions were both   ≤   7.8% for prucalopride and IS, and the average intra- and inter-day accuracies ranged from −3.0% to 8.5%. Extraction recoveries at three levels QC concentrations were in the range of 90.0–110.0% for prucalopride and 99.6% for IS. Matrix effects were found to be acceptable. The validated assay was successfully applied to a pharmacokinetic study of prucalopride following oral administration of 0.25, 0.5, 1.0   mg/kg to female and male rats respectively.

研究领域: 分析化学 · 药物代谢动力学 · 医学
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JOURNAL OF CHROMATOGRAPHY B-ANALYTICAL TECHNOLOGIES IN THE BIOMEDICAL AND LIFE SCIENCES · 2021 · IF 3.205

Pharmacokinetic and metabolomics approach based on UHPLC-MS to evaluate therapeutic effect of lignans from S. Chinensis in alzheimer's disease

Yuan Zhou,Mengying Wei,Meiling Fan,Zhongying Liu,Aimin Wang,Yuanyuan Liu,Lihui Men,Zifeng Pi,Zhiqiang Liu,Fengrui Song

Lignans from Schisandra chinensis (Turcz.) Baill (LFS) has been proved to improve impaired cognitive ability thereby show potential in treating Alzheimer’s disease (AD). In this study, UHPLC-Q-TOF-MS and UHPLC-QQQ-MS were adopted cooperatively to establish a method synchronously detecting 10 kinds of LFS monomers in rat plasma samples. And this method was further applied for pharmacokinetic study to compare the metabolism of LFS in normal and AD rats. The results indicated that AD rats showed an observably better absorption of LFS compared to normal rats. Based on time-varying plasma concentration of LFS, metabolomics was used to establish a plasma concentration–time-endogenous metabolite connection. In total 54 time-varying endogenous metabolites were screened and most of which were closely associated with AD. And LFS exerted a concentration dependent regulating effect to most of these metabolites. Through biomarker related pathways and biological function analysis, LFS might treat AD through neuroprotection, antioxidant damage and regulating the metabolism of unsaturated fatty acids. This is the first study connecting LFS absorbtion and endogenous metabolite changes with the time lapse. The pharmacokinetics and metabolic profile differences between normal and AD rats were firstly investigated as well. This study provides a novel perspective in exploring the effect and mechanism of LFS in treating AD.

CAS / MDL: 506-32-1 63-91-2
研究领域: 神经科学 · 药物代谢研究 · 中药学
✓ 已验证 产品关联 DOI PubMed 高影响因子
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MOLECULES · 2018 ·Vol. 23 ·期 8 ·1926 · IF 3.098

Simultaneous Analysis of 20 Mycotoxins in Grapes and Wines from Hexi Corridor Region (China): Based on a QuEChERS–UHPLC–MS/MS Method

Bo Zhang,Xia Chen,Shun-Yu Han,Min Li,Teng-Zhen Ma,Wen-Jun Sheng,Xia Zhu

The aim of this study is to develop and validate an improved analytical method for the simultaneous quantification of 20 types of mycotoxins in grapes and wines. In this research, the optimization of tandem mass spectrometer (MS/MS) parameter, ultra-high pressure liquid chromatography (UHPLC) separation, and QuEChERS procedure, which includes wine/water ratio, the amount and type of salt, clean-up sorbent, were performed, and the whole separation of mycotoxins was accomplished within 7 min analyzing time. Under optimum conditions, recoveries ranged from 85.6% to 117.8%, while relative standard deviation (RSD) remained between 6.0% and 17.5%. The limit of detection (LOD, 0.06–10 μg/L) and the limit of quantification (LOQ, 0.18–30 μg/L) were lower than those permitted by legislation in food matrices, which demonstrated the high sensitivity and applicability of this efficient method. Finally, 36 grapes and 42 wine samples from the Hexi Corridor region were analyzed. Penicillic acid (PCA), mycophenolic acid (MPA), cyclopiazonic acid (CPA), fumonisin B1 (FB1) and zearalenone (ZEN) were detected in a small number of grape samples with lower concentrations between 0.10 μg/L and 81.26 μg/L. Meanwhile, ochratoxin A (OTA), aflatoxin B2 (AFB2), MPA, CPA, and ZEN were detected in some wine counterparts with concentrations ranged from 0.10 μg/L to 4.62 μg/L. However, the concentrations of the detected mycotoxins were much lower than the maximum legal limits set of other products.Keywords:QuEChERS;UHPLC–MS/MS;mycotoxins;grapes and wines;hexi corridor region

研究领域: 食品科学 · 分析化学 · 农业化学
✓ 已验证 产品关联 DOI PubMed 高影响因子
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Food Chemistry-X · 2024 · IF 6.5

Based on theoretical design simultaneous analysis of multiple neonicotinoid pesticides in beeswax by deep eutectic solvents extraction combined with UHPLC-MS/MS

Guodong Mu,Sha Yan,Fei Pan,Haitao Xu,Xu Jing,Xiaofeng Xue

Beeswax, an FDA-approved component, has been extensively applied in feed, pharmaceutical, and food industries. The occurrence of neonicotinoid pesticides in beehive systems and their residues in beeswax have caused safety risks. Therefore, establishing a detection method for neonicotinoid pesticide residues in beeswax is crucial for ensuring its quality. The superhydrophobic property of beeswax makes it a challenge to develop suitable determination methods. In this work, we determined Proline and Oxalic acid as a suitable deep eutectic solvent (DES) to extract neonicotinoids from beeswax through theoretical design and verification tests. Systematic molecular dynamics simulations confirmed that hydrogen bonding and van der Waals forces facilitate the migration of neonicotinoid pesticides from beeswax into the DES. Performance analysis of the method revealed that the DES extraction combined with UHPLC-MS/MS approach exhibited excellent detection capabilities. It was applied to real beeswax sample analysis with the characteristics of simpleness, quickness, environmental friendliness, and high throughput.

研究领域: 分析化学 · 食品安全 · 环境科学
✓ 已验证 产品关联 DOI PubMed 高影响因子
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MICROCHEMICAL JOURNAL · 2020 · IF 3.594

Facile preparation of a magnetic porous organic frameworks for highly sensitive determination of eight alkaloids in urine samples based UHPLC-MS/MS

Kai Hu,Tiantian Pang,Yanmei Shi,Jiamin Cheng,Yanjie Huang

In this work, a facile strategy for the preparation of magnetic porous organic framework (Ni@POFs) was proposed by the reduction of Ni ions on its skeleton in situ. The properties of the material were confirmed by X-ray diffraction, vibrating sample magnetometer, infrared spectroscopy, transmission electron microscopy and scanning electron microscopy. The prepared Ni@POFs exhibits a strong magnetism and high extraction efficiency for targeted alkaloids. All the key factors that affect the extraction/desorption efficiency of the alkaloids onto the Ni@POFs material, such as sorbent amount, extraction time, sample pH and desorption condition, were investigated with the help of response surface methodology. In combination with magnetic solid phase extraction and ultra performance liquid chromatography-tandem mass spectrometry analysis, a novel method for the quantitative analysis of alkaloids in urine samples was proposed. The limits of detection and limits of quantitation for the eight alkaloids were found to be in the range of 0.9–6.0 and 3.0–20 pg mL −1 , respectively. The recoveries of spiked urine samples were in the range of 93.5–99.2% with RSDs less than 6.9%. The proposed method was successfully applied to analyze the metabolites in patient’s urine after the oral administration of berberine.

研究领域: 分析化学 · 药理学
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MOLECULES · 2019 ·Vol. 24 ·期 17 ·3057 · IF 3.06

Simultaneous Quantification and Pharmacokinetic Study of Nine Bioactive Components of Orthosiphon stamineus Benth. Extract in Rat Plasma by UHPLC-MS/MS

Zili Guo,Bo Li,Jinping Gu,Peixi Zhu,Feng Su,Renren Bai,Xianrui Liang,Yuanyuan Xie

Orthosiphon stamineusBenth. (OS) is a traditional folk medicine for the treatment of kidney stones and other urinary tract diseases. In this study, a rapid and sensitive Ultra high-performance liquid chromatography (UHPLC)-MS/MS approach was established and validated for the simultaneous quantification of nine bioactive components in rat plasma. The nine components from OS extract detected in rat plasma were danshensu, protocatechuic acid, caffeic acid, rosmarinic acid, salvianolic acid A, salvianolic acid B, cichoric acid, sinensetin and eupatorin. After liquid-liquid extraction with ethyl acetate, the plasma samples were subjected to a triple quadrupole mass spectrometer employing electrospray ionization (ESI) technique and operating in multiple reaction monitoring (MRM) with both positive and negative ion modes. The standard curves showed good linear regression (r> 0.9915) over the concentration range for the nine analytes. The inter-day and intra-day precision and accuracy were found to be within 15% of the nominal concentration. The recovery and stability of nine compounds were all demonstrated to be within acceptable limits. The approach was successfully applied to investigate the pharmacokinetic analysis of the nine bioactive components after oral administration of OS extract in rats.Keywords:Orthosiphon stamineusBenth.;bioactive constituents;UHPLC-MS/MS;rat plasma;pharmacokinetic study

CAS / MDL: 56-75-7 64-18-6
研究领域: 药理学 · 分析化学 · 传统医学
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ANALYTICAL LETTERS · 2024 · IF 1.6

Quality Evaluation of Calyx of Diospyros Kaki Thunb. by Ultra-High Performance Liquid Chromatography – Mass Spectrometry (UHPLC-MS) Profiling and Fingerprinting and Chemometrics

Anlan Yang,Xuexia He,Yanjuan Zhai,Chao Gu,Yujing Zhang,Song Li,Shengjun Chen,Xiachang Wang,Yuntian Zhang

Calyx of Diospyros kaki Thunb. (DKC), a famous traditional Chinese medicine, has a remarkable therapeutic effect on hiccups but its quality control is insufficient. In the study, a method was established by ultra-high performance liquid chromatography – mass spectrometry (UHPLC-MS). 17 peaks were observed in the mass spectrum and their chemical structures were preliminarily identified, including 3 organic acids and 14 flavonoids. The reference UHPLC fingerprint was built based on 25 batches of DKC samples, containing 15 common peaks. 11 batches of DKC samples from Guangxi and Hebei were superior to other 14 batches, sharing high similarity from 0.966 to 0.988 with the reference fingerprint. The chemometric methods, including hierarchical clustering analysis (HCA), principal component analysis (PCA), and partial least squares discriminant analysis (PLS-DA), were used to distinguish the DKC samples. The recognition methods clearly distinguished the medicinal materials from different regions, indicating that the main chemical constituents leading to the differences were protocatechuic acid, 4-hydroxybenzoic acid, rutin (presumptive result based on MS data), isoquercitrin, kaempferol, and hyperoside. The established fingerprint method is simple, rapid, repeatable, and specific and provides a reference for the quality evaluation of DKC.

CAS / MDL: 64-18-6
研究领域: 中药学 · 分析化学
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JOURNAL OF CHROMATOGRAPHY B-ANALYTICAL TECHNOLOGIES IN THE BIOMEDICAL AND LIFE SCIENCES · 2021 · IF 3.205

Determination of six parabens in biological samples by magnetic solid-phase extraction with magnetic mesoporous carbon adsorbent and UHPLC-MS/MS

Qianchun Zhang,Yongzhi Zhi,Linchun Bao,Yuguo Zheng,Xingyi Wang,Li Jiang,Yun Wu

Although parabens are useful due to their antiseptic properties, their widespread use has caused concerns regarding their potential toxicological effects. In this study, a novel magnetic solid-phase extraction combined with ultra-high-performance liquid chromatography-tandem mass spectrometry (MSPE-UHPLC-MS/MS) was developed, based on ordered magnetic mesoporous carbon (MMC), for paraben analysis. The MMC was prepared by soft-template synthesis, with a unique pore structure and a highly specific surface response, indicating potential as an excellent adsorbent. Several parameters affecting the paraben extraction efficiency were investigated and a novel method for paraben analysis in serum and urine samples using MSPE-UHPLCMS/MS was developed. The concentrations of methylparaben, ethylparaben, isopropylparaben, and propylparaben in these samples were 0.0380–4.36, 0.460–9.65, 0.0118–0.770, and 0.0363–0.641 μg/L, respectively, whereas isobutylparaben and butylparaben were not detected. Furthermore, satisfactory recoveries of 76.4–121% with relative standard deviations (n = 5) of 1.9–8.6% were obtained. Therefore, the developed MSPE-UHPLC-MS/MS method was efficient, highly sensitive, and reliable for analysing parabens in complex biological samples.

研究领域: 分析化学 · 环境科学 · 毒理学
✓ 已验证 DOI PubMed 高影响因子
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MICROCHEMICAL JOURNAL · 2024 · IF 4.9

Facile and fast fabrication of magnetic molecularly imprinted polymer for extraction of carbamazepine from environmental samples and fish tissues followed by UHPLC-MS/MS detection

Simin Zhuang,Dan Li,Yujun Liu,Chaomei Xiong

A rapid synthesis of carbamazepine (CBZ) magnetic molecularly imprinted polymer (MMIP) was proposed based on reflux precipitation polymerization method. The synthesis time for the formation of MIP coating on MMIP was shortened to less than 4 h. The characterization of MMIP demonstrates the successful synthesis of the imprinted layer. The adsorption selectivity of MMIP was systematically evaluated and showed fast selective recognition for CBZ. The MMIP based magnetic solid-phase extraction (MSPE) combined with UHPLC-MS/MS was developed, and its feasibility was validated in four complex matrices of environmental water, sediment, fish muscle and liver. It was successfully applied for the analysis of environmental water, sediment, and different fish tissues. Four environmental water samples from different sampling sites were found to contain CBZ at concentrations < LOD or LOQ, while the sediment samples collected at the same location did not contain CBZ. Two out of three wild snakeheads were found to contain CBZ, and the liver showed the highest residue. The study of drug exposed snakeheads indicate CBZ tends to accumulate in liver, followed by brain, heart and kidneys, and finally muscle and gills. The proposed method displays high potential for analyzing CBZ in complex environmental and biological samples.

研究领域: 分析化学 · 环境科学
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