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Fast determination of five chiral antipsychotic drugs using dispersive liquid–liquid microextraction combined with capillary electrophoresis
Analytical Methods ( IF 2.7 ) Pub Date : 2020-03-19 , DOI: 10.1039/c9ay02776a
Ming-Mu Hsieh, Tai-Chia Chiu, Szu-Hua Chen

This study developed a new method for the extraction, clean up, chiral separation, and determination of five pairs of phenothiazine drugs using ultrasound-assisted dispersive liquid–liquid microextraction combined with capillary electrophoresis (CE). A mixture of extraction solvent (30 μL of CHCl3) and dispersive solvent (200 μL of tetrahydrofuran) was rapidly injected using a syringe, which formed tiny cloudy droplets of an organic extractant that dispersed entirely into the aqueous phase. After centrifuging, the sediment phase of volume 60 ± 0.5 μL was transferred into a small vial and evaporated to dryness. The residue was reconstituted in 5 μL of aqueous solution, analyzed using CE and then successfully baseline separated in 6 min using a background electrolyte composed of 5 mM hydroxypropyl-γ-cyclodextrin, 0.9% poly(diallyldimethylammonium chloride), and 150 mM tris-formate at pH 3.0. The developed method was linear in the 0.01–10 μM range, with R2 ≥ 0.9956 for all target analytes. The limit of detection (S/N = 3) and the limit of quantification (S/N = 10) were 2–4 nM and 10 nM, respectively. Excellent repeatability (RSD ≤ 5.5%, n = 5) was achieved. The recoveries of all phenothiazine drugs from urine were in the 83.5–104.0% range. The advantages of this approach were low cost, versatility, simplicity, and high sensitivity.

中文翻译:

分散液-液微萃取结合毛细管电泳快速测定五种手性抗精神病药

这项研究开发了一种新方法,采用超声辅助分散液-液微萃取结合毛细管电泳(CE)来提取,纯化,手性分离和测定五对吩噻嗪类药物。萃取溶剂的混合物(30μLCHCl 3)并使用注射器快速注入分散溶剂(200μL四氢呋喃),形成有机萃取剂的细小混浊液滴,完全分散到水相中。离心后,将体积为60±0.5μL的沉淀相转移到一个小瓶中,并蒸发至干。将残留物重新溶解在5μL水溶液中,使用CE分析,然后使用5 mM羟丙基-γ-环糊精,0.9%聚二烯丙基二甲基氯化铵和150 mM三甲酸酯组成的背景电解质在6分钟内成功进行基线分离在pH 3.0下。所开发的方法在0.01–10μM范围内呈线性,R 2所有目标分析物均≥0.9956。检测限(S / N = 3)和定量限(S / N = 10)分别为2-4 nM和10 nM。获得了极好的重复性(RSD≤5.5%,n = 5)。尿液中所有吩噻嗪类药物的回收率在83.5–104.0%范围内。这种方法的优势是低成本,多功能性,简单性和高灵敏度。
更新日期:2020-04-24
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