JOURNAL OF PHARMACEUTICAL AND BIOMEDICAL ANALYSIS
·
2025
·
IF 3.1
Yi Qin,Xiaojun Guan,Shichao Zhang,Zijie Zhang,Chenrong Huang,Liyan Miao
Almonertinib and anlotinib are tyrosine kinase inhibitors used to treat malignant tumors, with their combination currently applied to non-small cell lung cancer (NSCLC) patients. This study aimed to develop a simple and rapid UPLC–MS/MS method for simultaneously detecting almonertinib, its active metabolite HAS-719, and anlotinib in human plasma. The analytes were separated on a Waters HSST3-C18 column following protein precipitation with acetonitrile. Mass detection was performed on a Waters TQS triple quadrupole mass spectrometer under positive electrospray ionization mode. The MRM ions were m/z 526.5→71.96 for almonertinib, m/z 512.4 → 455.41 for HAS-719, m/z 408.16→ 339.03 for anlotinib and m/z 518.5→372.26 for d6-HAS-000719 (internal standard). Method validation followed FDA guidelines and Chinese Pharmacopoeia regulations, demonstrating acceptable accuracy, precision, matrix effects, recovery, and stability. The method showed excellent linearity over 0.5–500 ng/mL for all three analytes, with correlation coefficients (r²)≥ 0.99. The validated UPLC-MS/MS method successfully monitored almonertinib and anlotinib concentrations in clinical, particularly for NSCLC patients.
研究领域:
药理学
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临床医学
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肿瘤学
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产品关联
DOI
PubMed
高影响因子
JOURNAL OF PHARMACEUTICAL AND BIOMEDICAL ANALYSIS
·
2019
·
IF 2.983
Ting Tai,Huan Zhou,Ting Zhu,Yu-Meng Jia,Jin-Zi Ji,Yi-Fei Li,Qiong-Yu Mi,Hong-Guang Xie
Vicagrel is a promising novel antiplatelet drug. However, the quantification of vicagrel in plasma is currently unavailable since it is liable to be hydrolyzed in plasma by esterases. In this study, an optimized strategy was developed and validated to stabilize vicagrel, 2-oxo-clopidogrel (thiolactone metabolite), and H4 (active thiol metabolite) before quantification of the analytes, such as addition of citric acid (for plasma acidification) and NaF (a non-specific esterase inhibitor) to inhibit esterase activity, immediate addition of a thiol-alkylating reagent MPB into blood samples to derivatize H4 for the formation of stable H4 derivative (i.e., MP-H4), use of the anticoagulant K 2 EDTA to minimize the conversion of 2-oxo-clopidogrel to H-endo, and keeping the analytes at 4 °C or on wet ice to minimize degradation of the analytes when processed and analyzed. The stability was measured as percent of each analyte remained in plasma samples after their storage for 4 h at 4 °C or in blood samples after 1 h at 4 °C. The results indicated that stability of vicagrel was increased significantly in stabilized plasma or blood samples compared with non-stabilized controls for rats and humans, respectively, and that the stability of 2-oxo-clopidogrel was increased to a certain extent. In contrast, MP-H4 formed was stable in plasma immediately after thorough mixture of MPB with blood. We conclude that the above strategy is useful for improving the stability of vicagrel, 2-oxo-clopidogrel, and H4 in rat or human plasma, and that vicagrel and its two major metabolites can be quantified accurately and simultaneously.
研究领域:
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
Frontiers in Chemistry
·
2022
·
IF 5.545
Shen Qing,Wang Haixing,Quan Bin,Sun Xiuhua,Wu Guohua,Huang Darong,Wang Qingcheng,Luo Pei
Salvia miltiorrhiza Bunge (SMB) has unambiguous biological functions in cardiovascular diseases, thus has been processed into different medicine forms. However, universal analytical method for fast quantification of bioactive compounds in SMB and SMB derived products is still missing. In this study, a polarity switching strategy was developed and optimized, which enabled the detection of the target compound in both positive and negative ion modes in a single run. The MS2 features of each compound were characterized to select the most prominent transitions for quantitative and qualitative analysis. Afterwards, the performance of this method was validated in terms of linearity (≥0.9916), limit of detection (LOD, 0.003–0.135 ngml−1), limit of quantification (LOQ, 0.010–0.450 ngml−1), precision (48.23 ± 2.58 ngml−1 to 53.72 ± 3.11 ngml−1), recovery (RSD 2.04%–5.79%), and stability (RSD ≤7.52%). Finally, the bioactive compounds in SMB and SMB derived products were determined, among which salvianate A, salvianolic acid A, and rosmarinic acid were the main components in all samples. In conclusion, the polarity switching UPLC-MS/MS method is efficient in accurate determining the bioactive compounds, which greatly shorten the time for analysis when compared with conventional methods. It has great potential quality control of SMB and SMB derived products.
研究领域:
药学
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分析化学
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产品关联
DOI
PubMed
高影响因子
American Journal of Translational Research
·
2021
·
IF 4.06
Shaochang Wu,Guidong Zhu,Dajin Zhou,Hongtao Xu,Longyou Zhao
Objective: This study was designed to demonstrate the accuracy of ultra-high performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS) in detecting serum concentration of anti-schizophrenic drugs in patients with mental illness. Methods: The study participants were 186 schizophrenia patients treated in our hospital. Serum concentrations of anti-schizophrenic drugs in Chinese patients with mental illness were evaluated according to the reference intervals of drug therapy recommended in the guidelines. Results: Five drugs, namely Aripiprazole (ARI), Amisulpride (AMI), Olanzapine (OLA), Paliperidone (PAL) and Ziprasidone (ZIP) all showed good linearity within the linear range. The within-day precision of the above five drugs was all between 1.3%-8.9% and the inter-day precision was between 1.8%-7.6%, with within-day and inter-day relative standard deviations (RSDs) less than 15.00% and accuracy ranging from 87.00% to 106.73%. However, AMI had a mean blood concentration of 436.31±241.05 ng/mL (median concentration: 379.34 ng/mL), which was significantly higher than the reference range (100-320 ng/mL) recommended in the guidelines. Good recovery rates (86.21%-99.77%) were obtained after the samples were stored at room temperature for 24 h, at 4°C for 48h and at -20°C for half a year. Conclusions: Given that UPLC-MS/MS renders more accurate results in detecting the concentration of psychotropic drugs, it can be applied clinically to detect the concentration of therapeutic drugs in patients with mental illness.
研究领域:
临床医学
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药理学
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产品关联
DOI
PubMed
高影响因子
JOURNAL OF CHROMATOGRAPHY B-ANALYTICAL TECHNOLOGIES IN THE BIOMEDICAL AND LIFE SCIENCES
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2019
·
IF 2.813
Yingyue Yi,Guanghui Ren,Ming Zheng,Di Zhao,Ning Li,Xijng Chen,Yang Lu
JJH201501, a deuterated modification for multi-target antidepressant vortioxetine, is currently in phase I clinical trial. This study aimed to establish a sensitive and rapid UPLC-MS/MS method that was capable of simultaneously detecting JJH201501 and its major metabolite JJH201501-01 quantitatively in human plasma. The pretreatment was achieved by protein precipitation using 4-fold(v:v) acetonitrile with 5 ng/mL fluoxetine as internal standard precipitant. For method validation, the method was investigated in terms of the selectivity, inter- and intra-run precision and accuracy, carryover, matrix effect, extraction recovery and stability. The total running time was 3 min, and the retention time of JJH201501 and JJH201501-01 was 1.17 min and 1.05 min, respectively. The linear concentration range for JJH201501 and JJH201501-01 was 0.2 to 50 ng/mL and 0.4 to 100 ng/mL, respectively. The results showed that this method was in line with the guidelines for bioanalytical method proposed by FDA. In addition, the method was successfully applied to a plasma pharmacokinetic study of JJH201501 tablets in healthy volunteers which was part of the phase I trial.
研究领域:
药物分析
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临床药理学
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分析化学
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DOI
高影响因子
JOURNAL OF CHROMATOGRAPHY B-ANALYTICAL TECHNOLOGIES IN THE BIOMEDICAL AND LIFE SCIENCES
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2018
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IF 2.441
Yao Li,Sheng Guo,Tingting Hua,Yanyan Wang,Dandan Wei,Ming Zhao,Shulan Su,Jin-ao Duan
The fruit of Ziziphus jujuba ( Jujubae Fructus ) has been used as food and crude drug for thousands of years. Although several chemical and biological studies have revealed triterpenic acid as the main bioactive constituent of Jujubae Fructus responsible for immune-regulatory activity, only few pharmacokinetic studies have been conducted. To comprehend the kinetics of triterpenic acids and promote their curative application, a sensitive and efficient ultra-performance liquid chromatography coupled with mass spectrometry method (UPLC-MS/MS) was established. UPLC-MS/MS was applied for the simultaneous determination of ceanothic acid, epiceanothic acid, pomonic acid, alphitolic acid, maslinic acid , betulinic acid , and betulonic acid in normal and immunosuppressed rat plasma samples. After sample preparation, chromatographic separation was performed on an Acquity UPLC BEH C 18 column (2.1 × 100 mm, 1.7 μm) with acetonitrile : methanol (1:1, v/v) and 0.5% ammonium acetate in water as mobile phase . The established method was validated and found to be specific, accurate, and precise for the seven triterpenic acids, and was successfully applied for the pharmacokinetic study of rat plasma samples. The results showed that the pharmacokinetic parameters (C max , T max , AUC 0–t , AUC 0–∞, and CLz/F) in the plasma samples of immunosuppressed rats were significantly different from those in normal rats, and might provide an insight for the clinical usage of triterpenic acids from Jujubae Fructus .
研究领域:
药理学
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分析化学
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中药学
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DOI
PubMed
高影响因子
Drug Testing and Analysis
·
2014
·Vol. 7
·期 2
·150-157
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IF 2.84
Xin Yao,Guisheng Zhou,Yuping Tang,Sheng Guo,Dawei Qian,Jin-ao Duan
Ginkgo biloba leaf extract has been widely used in dietary supplements and more recently in some foods and beverages. In addition to the well-known flavonol glycosides and terpene lactones, G. biloba leaves are also rich in nucleobases and nucleosides. To determine the content of nucleobases and nucleosides in G. biloba leaves at trace levels, a reliable method has been established by using hydrophilic interaction ultra performance liquid chromatography coupled with triple-quadrupole tandem mass spectrometry (HILIC-UPLC-TQ-MS/MS) working in multiple reaction monitoring mode. Eleven nucleobases and nucleosides were simultaneously determined in seven min. The proposed method was fully validated in terms of linearity, sensitivity, and repeatability, as well as recovery. Furthermore, hierarchical clustering analysis (HCA) was performed to evaluate and classify the samples according to the contents of the eleven chemical constituents. The established approach could be helpful for evaluation of the potential values as dietary supplements and the quality control of G. biloba leaves, which might also be utilized for the investigation of other medicinal herbs containing nucleobases and nucleosides. Copyright © 2014 John Wiley & Sons, Ltd.
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
MICROCHEMICAL JOURNAL
·
2021
·
IF 4.821
Jing Zhao,Jingjing Pu,Xiaopeng Wu,Boyu Chen,Yan He,Yue Zhang,Bingjun Han
Matrix effect (ME) is a critical factor that can significantly compromise the accuracy of pesticide residue analyses performed using ultra-performance liquid chromatography–tandem mass spectrometry (UPLC-MS/MS). In this study, five pesticides of different types, namely difenoconazole (triazoles), chlorpyrifos (organophosphates), thiram (dithiocarbamates), carbaryl (carbamates), and pyraclostrobin (strobilurins), were selected to investigate the UPLC-MS/MS MEs in five typical tropical fruits. The MEs and possible mechanisms of the main influence factors, i.e., pH value and sugar content, were studied for the pesticide residues in the tropical fruits. The proposed method was validated in terms of linearity, limit of detection (LOD), recovery, and precision. In the range of 0.005–0.5 μg mL −1 , the coefficients of determination (r) were better than 0.999, while the LODs and recoveries ranged from 0.16 to 4.4 μg kg −1 and from 75% to 120%, respectively. Results show that among the five typical tropical fruits, the ME was largest in longan, followed by that in banana; pineapple and guava showed lower MEs than those in banana, whereas papaya had the lowest. Chlorpyrifos has the largest ME, followed by thiram and difenoconazole, and the other pesticides have very small MEs. Moreover, the MEs can be reduced by adjusting the pH value and sugar content of the sample matrix. This study can be applied to assess the influence of MEs on the analysis results.
研究领域:
分析化学
·
食品科学
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产品关联
DOI
高影响因子
JOURNAL OF FOOD COMPOSITION AND ANALYSIS
·
2023
·
IF 4.3
Ling Li,Ping Li,Shi Tang,Caiju Xiao,Yukun Huang,Lijun Wang,Xiao Yang,Xianggui Chen,Bing Shao
An ultra-performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS) method was established for the simultaneous analysis of acrylamide (AA), 5-hydroxymethylfurfural (HMF), and heterocyclic aromatic amines (HAAs). A good separation of nine analytes was achieved within 15 min. Correlation coefficients (R 2 >0.9995) of the nine compounds were obtained within their respective linear ranges. The method also possessed low limits of detection (0.3 ng/mL for IQ, Norharman, 7,8-DiMeIQ, 10.00 ng/mL for MeIQ, 5-HMF, 0.05 ng/mL for PhIP, Phe-P-1, 0.10 ng/mL for Harman, 20.00 ng/mL for AA) and limits of quantification (15.00 mg/kg for IQ, Norharman, 7,8-DiMeIQ, 450.00 mg/kg for MeIQ, 3.00 mg/kg for PhIP, Phe-P-1, 300.00 mg/kg for 5-HMF and 750.00 mg/kg for AA). The method developed for the determination of samples commonly found among Sichuan cuisine, and fast food had good precision (RSD<9%) and recovery (83%-113%). This study provides a basis for the simultaneous rapid determination of nine chemical contaminants commonly found in thermally processed meat products and provides a technical reference for the simultaneous rapid determination of more chemical contaminants in thermally processed meat products.
研究领域:
分析化学
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食品科学
·
毒理学
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产品关联
DOI
高影响因子
PHYTOMEDICINE
·
2021
·
IF 5.34
Kaihui Zhang,Yufeng Yao,Meiqi Wang,Fangle Liu,Qian Wang,Huanhuan Ma,Yuanyuan Xie,Yunxia Ma,Pengyu Dai,Chenchen Zhu,Chaozhan Lin
Background Rabdosia Serra, the dried aerial parts of Rabdosia serra (Maxim.) Hara (RS) from the Labiatae family, is a traditional Chinese herbal medicine called Xihuangcao. Although RS has been found to exert a therapeutic effect on cholestasis, the underlying molecular mechanism remains unclear. Purpose This study was designed to investigate the pharmacological effect and mechanism of RS on cholestatic rats using metabolomics platform. Methods Histopathology and biochemical evaluations were performed to determine the therapeutic effect of RS and developed a rapid metabolite detection technology method based on UPLC-MS/MS to perform metabolomics research. Further, quantitative real-time polymerase chain reaction (RT-qPCR) was used to study the effect of RS on the bile acid metabolism pathway at the transcriptional level. Results RS significantly reduced the bile flow rates in cholestatic rats and decreased the levels of ALT, AST, TBA, T-BIL, and LDH, which were increased in the model group. Histological analysis showed that RS alleviated the liver injury induced by ANIT. Serum metabolomics results revealed 33 of the 37 biomarkers were found to be significantly altered by ANIT, and 26 were considerably changed following treatment with RS. Metabolic pathway analysis revealed four pathways such as primary bile acid biosynthesis, biosynthesis of unsaturated fatty acids, and arachidonic acid and tryptophan metabolism. The bile acid secretion process and the inflammation and oxidative stress processes are the major biochemical reactions following treatment with ANIT and RS. Bile acid-targeted metabolomics study showed that TCA, GCA, GCDCA, and GDCA might be sensitive biomarkers that induced liver injury. we found that treatment with RS regulated the levels of bile acid in the serum and liver and restored the proportion of bile acids, especially CA and conjugated bile acids, such as TCA and GCA, in the bile duct. RS increased the mRNA expression levels of FXR, SHP, BSEP , and MRP2 in livers, and IBABP, OST-α , and OST-β in the ileum. Conclusion : In this study, RS was found to protect the liver by regulating multiple metabolic pathways and promoting the excretion of bile acids. Simultaneously, RS played an essential role in reversing the imbalance of bile acids and protected against cholestasis by regulating the expression of transporters associated with bile acids. We demonstrated the correlation between molecular mechanisms and metabolites, provide a reference for the fabrication of extracts that can be used to treat cholestasis.
研究领域:
药理学
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代谢组学
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传统中药
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肝脏疾病
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产品关联
DOI
PubMed
高影响因子
JOURNAL OF PHARMACEUTICAL AND BIOMEDICAL ANALYSIS
·
2019
·
IF 2.983
Chengcan Lu,Kejia Fu,Kangna Cao,Jiali Wei,Jing Zhou,Di Zhao,Ning Li,Yang Lu,Xijing Chen,Yongjie Zhang
A rapid and sensitive ultra-high-performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS) method was applied to investigate the permeability characteristics and transport mechanism of trihexyphenidyl hydrochloride (TH) in D-hanks with the Caco-2 cells model. Analytes were separated using an Zorbax Extend-Agilent C 18 (1.8 μm, 4.6 × 30 mm) column following a simple methanol precipitation treatment. The mobile phase consisted of methanol and water containing 0.1% formic acid, and the total gradient program time was 1.5 min. Method validation results showed TH was linear in 2–500 ng/mL (r 2 > 0.99), and the lower limit of quantification (LLOQ) was 2 μg/mL. The intra-run and inter-run precision (coefficient of variation, CV) was within 2.80%, and the accuracy (relative error, RE) was within ±11.10%. Stability of TH was evaluated in different storage conditions, including short-term I-III, long-term I-III, 2 and 4 h in the artificial gastrointestinal tract, respectively. There was no obvious interference between TH and internal standards (IS). With the established Caco-2 monolayer permeability model, Papp(AB) of TH was calculated as 46.29 ± 8.31 × 10 −6 cm/s, and the efflux ratio (ER) value was calculated as 0.22, indicating a high permeability character of TH. The transmembrane transport of TH followed the concentration-dependent, temperature-independent, and energy-free manner. Collectively, these characteristics indicate that TH is a highly permeable drug and the transport mechanism is mainly via passive diffusion.
研究领域:
药理学
·
药物代谢动力学
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产品关联
DOI
PubMed
高影响因子
ENVIRONMENTAL SCIENCE AND POLLUTION RESEARCH
·
2021
·Vol. 29
·期 15
·21826-21838
·
IF 4.223
Pang Xiuyu,Li Chenyu,Zang Chuanjiang,Guan Lei,Zhang Peng,Di Chunxiang,Zou Nan,Li Beixing,Mu Wei,Lin Jin
An analytical method of simultaneous detection of ten insecticide residues in honey and pollen was established. The samples were purified with QuEChERS approach using new adsorbents and analyzed with UPLC-MS/MS. The results showed that both of graphene and carbon nanotubes were highly efficient adsorbents for the dSPE clean up to eliminate coextractives in the samples, and graphene was superior to carbon nanotubes for the detection of pesticide residues in honey and pollen samples. The proposed method was used to detect pesticide residues in 25 honey samples and 30 pollen samples which were randomly collected from more than ten provinces in China. All honey samples contain 1–27 μg/kg of chlorpyrifos residues. Only 4% of the honey samples were detected containing acetamiprid and imidacloprid, while the other seven pesticides were not detected. Chlorpyrifos residues were found in all pollen samples (5–66 μg/kg), among which twenty percent exceeded the maximum residue limits (MRLs, 50 μg/kg, European Commission Regulation). Most of the pollen samples containing pesticide concentrations higher than MRLs were collected from rape, followed by lotus, camellia, and rose. Besides, 36.7% and 33.3% of the pollen samples had imidacloprid and flupyradifurone higher than 5 μg/kg. A total of 26.7% pollen samples were detected containing bifenthrin, while none of the other six pesticides were detected in pollen samples.
研究领域:
分析化学
·
食品科学
·
环境科学
✓ 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）