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基于正交设计优化中空纤维液相微萃取-高效液相色谱法测定大鼠血浆中木兰碱的药代动力学。

Orthogonal array design for optimization of hollow-fiber-based liquid-phase microextraction combined with high-performance liquid chromatography for study of the pharmacokinetics of magnoflorine in rat plasma.

机构信息

Department of Pharmacy, Urumqi General Hospital of PLA, Urumqi, Xinjiang 830000, China.

出版信息

Anal Bioanal Chem. 2012 Jun;403(7):1951-60. doi: 10.1007/s00216-012-6013-8. Epub 2012 May 5.

Abstract

In this work, a new sample-preparation method based on hollow-fiber liquid-phase microextraction (HF-LPME) was developed for analysis of magnoflorine in rat plasma. Analysis was accomplished by reversed-phase high-performance liquid chromatography (HPLC), with ultraviolet detection by use of a photodiode-array detector. An orthogonal array design (OAD) was found to be effective for optimization of major conditions which may affect the efficiency of HF-LPME. Under the optimized conditions (pH of donor and acceptor phases 12 and 2.0, respectively; extraction time 20 min; stirring speed 800 rpm; and addition of 10 % (w/v) salt), the preconcentration factor for magnoflorine was 355. Calibration curves with reasonable linearity (r(2)≥0.9994) were obtained in the range 10-1000 ng mL(-1). Intra-day and inter-day precision (RSD) were <5.5 % and the limit of detection (LOD) for the analyte was 3.0 ng mL(-1) (S/N=3). The validated method was successfully used for pharmacokinetic studies of magnoflorine in rat plasma after intravenous administration.

摘要

本工作建立了一种基于中空纤维液相微萃取(HF-LPME)的新型样品前处理方法,用于大鼠血浆中美防己碱的分析。采用反相高效液相色谱(HPLC)法,紫外检测,二极管阵列检测器检测。正交试验设计(OAD)被发现可有效优化可能影响 HF-LPME 效率的主要条件。在优化条件下(供体相和受体相的 pH 值分别为 12 和 2.0;萃取时间 20 min;搅拌速度 800 rpm;添加 10%(w/v)盐),美防己碱的预浓缩因子为 355。在 10-1000 ng mL(-1)范围内,获得了具有合理线性(r(2)≥0.9994)的校准曲线。日内和日间精密度(RSD)均<5.5%,分析物的检测限(LOD)为 3.0 ng mL(-1)(S/N=3)。该验证方法成功用于大鼠静脉注射美防己碱后的药代动力学研究。

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