BIOMEDICAL CHROMATOGRAPHY
·
2025
·Vol. 39
·期 2
·e6070
·
IF 1.7
Li Li,Dan Yu,Wen-Fei Sun,Qi-Zhong Jin,Xing-Jie Chang,Qian Shi
Ginkgolide B (GB) is the main active ginkgolide in Ginkgo biloba leaves extract. Pharmacological study suggested that GB exhibits protective effect on nervous system impaired and can be used in the treatment of dementia, cerebral insufficiency or related cognitive decline. However, the information on pharmacokinetics of GB in vivo was limited. In this study, a sensitive LC–MS/MS analytical method was developed to accurately determinate the concentration of GB in dog plasma and applied to the pharmacokinetic study of GB in dogs after bolus injection of GB. A portion of 100 μL dog plasma was pretreated by liquid–liquid extraction using 1 mL of ethyl acetate. The GB and IS were separated on a Waters ACQUITY HSS T3 column using acetonitrile and water containing 0.1% formic acid as mobile phase, at a flow rate of 0.4 mL/min. Multiple-reaction monitoring (MRM) mode was used for quantitative analysis of GB and tolbutamide (internal standard) in negative electrospray ionization. GB showed excellent linearity with correlation coefficient > 0.99 over the concentration range of 1–5000 ng/mL. The intra and interday RSD% were less than 7.4%, while the RE% ranged from −6.1% to 9.6%. The mean extraction recovery was > 83.1%. The validated method was further successfully applied to pharmacokinetic study of GB in dog plasma. Dose-proportional pharmacokinetics of GB were observed after bolus injection administration in dogs. This comprehensive study of the pharmacokinetics of GB in dogs will provide useful information for its further development in clinic.
研究领域:
药理学
·
分析化学
✓ 已验证
产品关联
DOI
PubMed
高影响因子
Frontiers in Pharmacology
·
2025
·
IF 4.8
Fengyichi Zhang,Fanxi Guo,Xinyu Zhao,Chongyang Li,Junli Wang,Mengyun Wang,Ruixia Ma,Baochang Chen,Qiangqiang Miao,Yimeng Wang,Zihan Wang,Di Cao,Zugong Yu
A rapid, sensitive and reliable ultra–performance liquid chromatography–tandem mass spectrometry (UPLC–MS/MS) was developed and validated for the simultaneous quantitation of pyrantel (PYR), praziquantel (PRA), febantel (FBT) and its active metabolites, fenbendazole (FEN) and oxfendazole (OXF) in dog plasma. Fenbendazole–D3 (FEN–D3) was used as an internal standard (IS). The analytes and IS were prepared using simple protein precipitation (PP) combined with liquid–liquid extraction (LLE). Chromatographic analysis was performed on UPLC BEH C18 column using acetonitrile–0.1% formic acid in water for gradient elution. Detection was carried out in multiple reaction monitoring (MRM) mode under positive electrospray ionization. The standard curves were linear through the concentration range of 4–240 ng/mL for PYR and OXF, 15–900 ng/mL for PRA, 2–120 ng/mL for FBT and 10–600 ng/mL for FEN with all correlation coefficients >0.99. The intra–and inter–batch precision was 1.08%–14.26% and accuracy was from 90.66% to 110.28%. The mean extraction recoveries for the analytes and IS were >90%. The total run time was 9.0 min. The developed method was successfully applied to a bioequivalence study after oral administration of compound febantel tablets in 38 healthy dogs.
研究领域:
兽医学
·
分析化学
✓ 已验证
产品关联
DOI
PubMed
高影响因子
MOLECULES
·
2015
·Vol. 20
·期 11
·20031-20041
·
IF 2.416
Jie Zhao,Ting Geng,Qi Wang,Haihong Si,Xiaoping Sun,Qingming Guo,Yanjing Li,Wenzhe Huang,Gang Ding,Wei Xiao
Ginkgolide B (GB), an important active constituent ofGinkgo bilobaextract, has been used in clinical applications for the treatment of dementia, cerebral insufficiency or related cognitive decline. To investigate the main pharmacokinetic characteristics of three different GB formulations in beagle dogs, a simple, specific and sensitive LC-MS/MS method was established and validated. The separation of the analytes was achieved on an Agilent Eclipse Plus C18column (1.8 μm, 2.1 × 50 mm) with a mobile phase consisting of water and acetonitrile. The flow rate was set at 0.4 mL/min. Quantitation was performed using multiple reaction monitoring (MRM) in negative ion mode, with the transitions atm/z(Q1/Q3) 423.1/367.1 for GB andm/z269.3/170.0 for IS. The linear calibration curve of GB was obtained over the concentration range of 2–200 ng/mL. The intra- and inter-day precisions were <15% and the accuracies were within ±12.7%. The validated method was applied to compare the pharmacokinetic characteristics of GB in healthy beagle dogs after oral administration of three formulations (HME08, GB capsule prepared by hot-melt extrusion technology; LL06, GB pellet prepared by liquid layer technology; conventional GB tablet). The Cmaxvalues of GB from different formulations in beagle dog plasma were 309.2, 192.4 and 66.6 µg/L, and the AUC values were 606.7, 419.1 and 236.2 µg/L·h, respectively. The data suggested that the exposure level of GB from HME08 and LL06 in beagle dog plasma was greatly improved compared with conventional tablets. This study should be helpful for the design and development of oral GB preparations.Keywords:ginkgolide B;hot-melt extrusion;liquid layer;beagle dog plasma;pharmacokinetics;LC-MS/MS
研究领域:
药理学
·
药物分析
·
生物化学
✓ 已验证
产品关联
DOI
PubMed
高影响因子
JOURNAL OF PHARMACEUTICAL AND BIOMEDICAL ANALYSIS
·
2024
·
IF 3.1
Tao Ke,Zhongyuan Zhao,Junhuan Lin,Fengting Ou,Kaikai Chen,Kui Zeng,Debo He,Shengqiang Tong,Xinyi Wang,Lushan Yu,Jing Chen
The aim of this study was to develop and fully validate a sensitive and rapid ultra-high performance liquid chromatography-tandem mass spectrometry (UHPLC-MS/MS) method for simultaneous quantification of pristinamycin ⅠA (PⅠA) and pristinamycin ⅡA (PⅡA) in plasma of beagle dogs after oral administration of pristinamycin tablets. PⅠA, PⅡA and quinupristin (internal standard, IS) were separated on an Agilent Eclipse Plus C 18 column (2.1 mm × 100 mm, 3.5 μm particle size) by using gradient elution consisting of methanol and water (0.1 % formic acid) at a flow rate of 0.4 mL/min in 4.0 min. Multiple reaction monitoring (MRM) mode was performed to quantify data under monitoring precursor-product ion transitions of m/z 867.6→134.1, 548.4→287.1 and 1022.7→133.9 for PⅠA, PⅡA and IS at positive ion mode, respectively. The method was developed at linearity ranging from 1.0 to 1000 ng/mL for all analytes.The accuracy of PⅠA and PⅡA was observed to range between −10.6 % and 7.1 %, while the precision was found to be within 8.9 %. No significant matrix effect was observed. PⅠA and PⅡA demonstrated stability during sample storage, preparation and analytic procedures. Furthermore, this method was successfully applied in the investigation of the pharmacokinetic profile of PⅠA and PⅡA in beagle dogs after oral administration of pristinamycin tablets (75 mg for PⅠA and 175 mg for PⅡA). The biological half-life (t 1/2 ) was determined to be 1.75 ± 0.07 h and 1.44 ± 0.31 h for PⅠA and PⅡA, respectively. The areas under curves (AUC 0-t ) of PⅠA and PⅡA were 80.7 ± 24.6 and 230 ± 94.8 μg/L·h, respectively.
研究领域:
分析化学
·
药理学
·
兽医学
✓ 已验证
产品关联
DOI
PubMed
高影响因子
JOURNAL OF CHROMATOGRAPHY B-ANALYTICAL TECHNOLOGIES IN THE BIOMEDICAL AND LIFE SCIENCES
·
2024
·
IF 2.8
Yunfeng Zhu,Fangkai Wang,Xin Wang,Ya Cheng,Xingyu Wang,Ali Fan,Jiawei Chang
Taletrectinib is a potent selective ROS and pan-NTRK tyrosine kinase inhibitor (TKI) and has been developed to treat non-small cell lung cancer (NSCLC). To facilitate pharmacokinetic and toxicokinetic studies of taletrectinib, we developed a procedure for ultra-high-performance liquid chromatography tandem mass spectrometry (UPLC-MS/MS) to detect the plasma level of taletrectinib in dogs. This assay procedure was validated in compliance with FDA guidance. The dog plasma samples were spiked with internal standard (IS), followed by protein precipitation, and analyzed using a Waters ACQUITY BEH C 18 column coupled to a Thermo triple quadrupole mass spectrometer. Separation was executed using the acetonitrile-0.1 % formic acid solution with gradient elution, at a flow rate of 0.4 mL/min. Taletrectinib and IS were monitored by multiple reaction monitoring (MRM) with m / z 406.2 > 349.2 and m / z 441.2 > 138.1, respectively. The procedure demonstrated excellent linearity with a correlation coefficient greater than 0.999 within the concentration range of 0.2–200 ng/mL. The inter- and intra-day accuracy ranged from −5.25 % to 5.26 %, and the precision was below 6.39 %. Acetonitrile-mediated protein precipitation showed high extraction efficiency and a recovery above 85 %. The procedure was then applied to quantify taletrectinib in beagle dog plasma after oral and intravenous doses and achieved success. The obtained pharmacokinetic parameters indicated high bioavailability of taletrectinib (>85 %) and extensive tissue distribution (>40 L/kg).
研究领域:
药理学
·
肿瘤学
·
分析化学
✓ 已验证
产品关联
DOI
PubMed
高影响因子
JOURNAL OF CHROMATOGRAPHY B-ANALYTICAL TECHNOLOGIES IN THE BIOMEDICAL AND LIFE SCIENCES
·
2025
·
IF 2.8
Wen Xiao,Haihui Ren,Yueyi Zhang,Jiameng Han,Qiaorong Liu,Zunjian Zhang,Yuan Tian
Free fatty acids (FFAs) play a key role in living organisms and participate in metabolic processes, mainly as a source of energy for cells. The C C position isomer of FFAs is strongly associated with many diseases, but quantification of its double bond position isomer remains a challenge in lipid analysis. In this study, based on the requirements of the pseudotargeted metabolomics, an analytical method based on a two-step derivatization LC-MS/MS method and a multiple reaction monitoring (MRM) mode was established and fully validated in terms of linearity, precision, and stability. The results demonstrated that the method relatively quantified 30 FFAs in plasma samples. These included 8 saturated fatty acids (SFAs), 12 monounsaturated fatty acids (MUFAs), and 10 polyunsaturated fatty acids (PUFAs). The developed method was applied to analyze the increase or down-regulation of the relative content of FFAs before and after the administration of the drug in Beagle dogs, which may help to explain the therapeutic effect of sacubitril valsartan. The establishment of this method allows the study of FFAs in Beagle dogs plasma to be no longer limited to analysis at the subclass level but can be focused at the isomer level.
研究领域:
代谢组学
·
脂质分析
·
质谱技术
·
药理学
·
临床研究
✓ 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）