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中空纤维液相微萃取结合高效液相色谱法测定生物体液中的痕量米格列奈。

Hollow fiber liquid-phase microextraction combined with high performance liquid chromatography for the determination of trace mitiglinide in biological fluids.

机构信息

School of Chemical Sciences, Universiti Sains Malaysia, 11800 Penang, Malaysia.

出版信息

J Chromatogr B Analyt Technol Biomed Life Sci. 2012 May 1;895-896:131-6. doi: 10.1016/j.jchromb.2012.03.031. Epub 2012 Mar 28.

Abstract

A hollow fiber liquid phase microextraction (HF-LPME) in conjunction with reversed phase HPLC-UV method was developed for the extraction and determination of trace amounts of the antidiabetic drug, mitiglinide (MIT) in biological fluids. The drug was extracted from 10 mL aqueous sample (donor phase (DP)) into an organic phase impregnated in the pores of hollow fiber, followed by the back extraction into a second aqueous solution (acceptor phase (AP)) located in the lumen of the hollow fiber. Parameters influencing the extraction efficiency including the kind of organic solvent, composition of DP and AP, extraction time, stirring rate and salt addition were investigated and optimized. Under the optimized extraction conditions, high enrichment factors (210-fold), good linearity (5-1000 ng mL(-1)) and detection limit lower than 1.38 ng mL(-1) were achieved. Recoveries of spiked samples were in the range (88.3-96.3%) and (92.0-99.3%) for urine and plasma samples, respectively. The percent relative standard deviation (n=9) for the extraction and determination of three concentration levels (100, 400 and 800 ng mL(-1)) of MIT were less than 10.6% and 13.6% for urine and plasma samples, respectively. The developed method is simple, sensitive and has been successfully applied to the analysis of MIT in biological fluids.

摘要

采用中空纤维液相微萃取(HF-LPME)与反相高效液相色谱-紫外检测法(HPLC-UV)联用,建立了一种从 10 mL 生物体液样品(水相样品(DP))中萃取痕量抗糖尿病药物米格列奈(MIT)并进行检测的方法。药物从 DP 转移到中空纤维内部孔道中的有机相中,随后通过反萃取进入位于中空纤维内腔的第二水相(接受相(AP))中。考察并优化了影响萃取效率的参数,包括有机溶剂的种类、DP 和 AP 的组成、萃取时间、搅拌速度和盐的添加等。在优化的萃取条件下,实现了高富集倍数(210 倍)、良好的线性范围(5-1000ng/mL)和检测限低于 1.38ng/mL。尿液和血浆样品中 MIT 的加标回收率分别在 88.3%-96.3%和 92.0%-99.3%的范围内。对于尿液和血浆样品中 MIT 的三个浓度水平(100、400 和 800ng/mL)的萃取和测定,相对标准偏差(n=9)小于 10.6%和 13.6%。所建立的方法简单、灵敏,已成功应用于生物体液中 MIT 的分析。

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