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A Simple and Sensitive HPLC-MS/MS Assay for the Quantitation of Blonanserin and N-Desethyl Blonanserin in Rat Plasma and Its Application to Pharmacokinetic Study
Journal of Analytical Methods in Chemistry ( IF 2.6 ) Pub Date : 2022-04-07 , DOI: 10.1155/2022/5914581
Shan-Qing Huang 1 , Xiao-Lin Li 1 , Zhan-Zhang Wang 1, 2 , Hao-Yang Lu 1, 2 , Tao Xiao 1 , Xiao-Jia Ni 1, 2 , Shu-Jing Liu 1 , Ming Zhang 1, 2 , De-Wei Shang 1, 2 , Yu-Guan Wen 1, 2
Affiliation  

A high-performance liquid chromatographic method coupled with triple quadrupole mass spectrometry (LC-MS/MS) for the analysis of blonanserin and its active metabolite, N-desethyl blonanserin, in rat plasma has been developed and validated. The biological samples were treated by simple direct protein precipitation before separation on an Agilent Eclipse Plus C18 column (4.6 × 100 mm, 3.5 μm) with a column temperature of 35°C at a flow rate of 0.5 mL/min. The mobile phase A is a mixture of methanol and water (75 : 25, v/v, 5 mM ammonium formate), and the mobile phase B is acetonitrile containing 0.1% formic acid. The ratio of mobile phase A to mobile phase B is 15 : 85. Electrospray ionization (ESI) multiple reaction monitoring modes are used for detection, which are m/z 368.10 ⟶ 296.90 (blonanserin), m/z 340.15 ⟶ 297.05(N-desethyl blonanserin), and m/z 348.15⟶ 302.05 (N-desethyl blonanserin-d8). The linear response range was 0.1–100.0 ng/mL for blonanserin and N-desethyl blonanserin. The lower limit of quantification (LLOQ), calibration curves, carryover, and matrix effects were sufficiently accurate and precise according to the National Medical Products Administration (NMPA) guidelines for bioanalytical method validation. This analytical method was successfully applied in a blonanserin-poloxamer thermosensitive gel pharmacokinetic study in rats.

中文翻译:

一种简单而灵敏的 HPLC-MS/MS 测定大鼠血浆中布南色林和 N-去乙基布南色林的定量及其在药代动力学研究中的应用

开发并验证了一种高效液相色谱法与三重四极杆质谱联用 (LC-MS/MS) 分析大鼠血浆中布南色林及其活性代谢物N-去乙基布南色林的方法。在使用 Agilent Eclipse Plus C 18色谱柱(4.6 × 100 mm,3.5  μm) 柱温为 35°C,流速为 0.5 mL/min。流动相 A 是甲醇和水的混合物(75 : 25,v/v,5 mM 甲酸铵),流动相 B 是含有 0.1% 甲酸的乙腈。流动相A与流动相B的比例为15:85。检测采用电喷雾电离(ESI)多种反应监测模式,m/z 368.10 ⟶ 296.90(布南色林),m/z 340.15 ⟶ 297.05( N -去乙基布南色林)和m/z 348.15⟶ 302.05(N-去乙基布南色林-d 8)。布南色林和N的线性响应范围为 0.1–100.0 ng/mL-去乙基布南色林。根据美国国家药品监督管理局 (NMPA) 生物分析方法验证指南,定量下限 (LLOQ)、校准曲线、交叉污染和基质效应足够准确和精确。该分析方法成功应用于布南色林-泊洛沙姆热敏凝胶在大鼠体内的药代动力学研究。
更新日期:2022-04-07
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