School of Chemical Sciences, Universiti Sains Malaysia, 11800 Minden, Penang, Malaysia.
School of Chemical Sciences, Universiti Sains Malaysia, 11800 Minden, Penang, Malaysia.
Talanta. 2015 Jan;131:590-6. doi: 10.1016/j.talanta.2014.08.037. Epub 2014 Aug 20.
A new analytical method for the simultaneous determination of the antidiabetic drugs rosiglitazone (ROS) and metformin hydrochloride (MH) with marked differences in their affinity towards organic solvents (log P of 2.4 and -1.43, respectively) was developed. Prior to the HPLC separation, the drugs were subjected to a sequential hollow fiber liquid phase microextraction (HF-LPME) procedure. Two sequential HF-LPME approaches were considered, the preferred one involves the use of two vials containing solution mixtures for the extraction of ROS (vial 1) and MH (vial 2), respectively, but using the same fiber and acceptor phase. Important parameters that affect the extraction efficiency such as extracting solvent, donor phase conditions, HCl concentration, agitation, extraction time, addition of salt, etc. were studied. Under the optimum conditions, good enrichment factors (EF, 471 and 86.6 for ROS and MH, respectively) were achieved. Calibration curves were linear over the range 1-500 (r(2)=0.998) and 5-2500 ng mL(-1) (r(2)=0.999) for ROS and MH, respectively. The relative standard deviation values (RSD%) for six replicates were below 8.4%. Detection and quantitation limits based on S/N ratio of 3 and 10 were 0.12, 1.0 and 0.36, 3.0 ng mL(-1) for ROS and MH, respectively. The proposed method is simple, sensitive and opens up new opportunities for the microextraction of analytes with contrasting properties.
一种新的分析方法用于同时测定具有显著不同有机溶剂亲和力的抗糖尿病药物罗格列酮（ROS）和盐酸二甲双胍（MH）（log P 分别为 2.4 和-1.43）。在 HPLC 分离之前，将药物进行顺序中空纤维液相微萃取（HF-LPME）程序。考虑了两种顺序 HF-LPME 方法，首选方法涉及使用两个含有溶液混合物的小瓶分别用于提取 ROS（小瓶 1）和 MH（小瓶 2），但使用相同的纤维和接受相。研究了影响萃取效率的重要参数，如萃取溶剂、供体相条件、HCl 浓度、搅拌、萃取时间、加盐等。在最佳条件下，实现了良好的富集因子（EF，ROS 和 MH 分别为 471 和 86.6）。ROS 和 MH 的校准曲线在 1-500（r(2)=0.998）和 5-2500 ng mL(-1)（r(2)=0.999）范围内呈线性。对于六个重复，相对标准偏差（RSD%）值低于 8.4%。基于 S/N 比为 3 和 10 的检测限和定量限分别为 0.12、1.0 和 0.36 ng mL(-1)，用于 ROS 和 MH。该方法简单、灵敏，为具有对比性质的分析物的微萃取开辟了新的机会。
