School of Chemical Sciences, Universiti Sains Malaysia, 11800 Penang, Malaysia.
J Chromatogr A. 2010 Jun 4;1217(23):3654-9. doi: 10.1016/j.chroma.2010.03.055. Epub 2010 Apr 4.
A three-phase hollow fiber liquid-phase microextraction (HF-LPME) coupled either with capillary electrophoresis (CE) or high performance liquid chromatography (HPLC) with UV detection methods was successfully developed for the determination of trace levels of the anti-diabetic drug, rosiglitazone (ROSI) in biological fluids. The analyte was extracted into dihexyl ether that was immobilized in the wall pores of a porous hollow fiber from 10 mL of aqueous sample, pH 9.5 (donor phase), and was back extracted into the acceptor phase that contained 0.1M HCl located in the lumen of the hollow fiber. Parameters affecting the extraction process such as type of extraction solvent, HCl concentration, donor phase pH, extraction time, stirring speed, and salt addition were studied and optimized. Under the optimized conditions (extraction solvent, dihexyl ether; donor phase pH, 9.5; acceptor phase, 0.1M HCl; stirring speed, 600 rpm; extraction time, 30 min; without addition of salt), enrichment factor of 280 was obtained. Good linearity and correlation coefficients of the analyte was obtained over the concentration ranges of 1.0-500 and 5.0-500 ng mL(-1) for the HPLC (r(2)=0.9988) and CE (r(2)=0.9967) methods, respectively. The limits of detection (LOD) and limits of quantitation (LOQ) for the HPLC and CE methods were (0.18, 2.83) and (0.56, 5.00) ng mL(-1), respectively. The percent relative standard deviation (n=6) for the extraction and determination of three concentration levels (10, 250, 500 ng mL(-1)) of ROSI using the HPLC and CE methods were less than 10.9% and 13.2%, respectively. The developed methods are simple, rapid, sensitive and are suitable for the determination of trace amounts of ROSI in biological fluids.
采用三相中空纤维液相微萃取（HF-LPME），分别与毛细管电泳（CE）或高效液相色谱（HPLC）与紫外检测法联用，成功建立了用于测定生物体液中痕量抗糖尿病药物罗格列酮（ROSI）的方法。在 pH 9.5 的水相（供体相）中，将分析物萃取到固定在多孔中空纤维壁孔中的二己基醚中，然后将其反萃取到位于中空纤维内腔的 0.1M HCl 接受相中。研究并优化了影响萃取过程的参数，如萃取溶剂的类型、HCl 浓度、供体相 pH 值、萃取时间、搅拌速度和加盐量。在优化条件下（萃取溶剂，二己基醚；供体相 pH 值，9.5；接受相，0.1M HCl；搅拌速度，600 rpm；萃取时间，30 min；不加盐），得到 280 的富集因子。在 HPLC（r²=0.9988）和 CE（r²=0.9967）方法中，分析物的线性范围和相关系数分别为 1.0-500 和 5.0-500 ng mL（-1）。HPLC 和 CE 方法的检测限（LOD）和定量限（LOQ）分别为（0.18、2.83）和（0.56、5.00）ng mL（-1）。使用 HPLC 和 CE 方法，在 10、250 和 500 ng mL（-1）三个浓度水平下，萃取和测定 ROSI 的相对标准偏差（n=6）分别小于 10.9%和 13.2%。所建立的方法简单、快速、灵敏，适用于生物体液中痕量 ROSI 的测定。
