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采用串联分散液液微萃取结合高效液相色谱法快速测定复杂基质中的某些精神药物。

Rapid determination of some psychotropic drugs in complex matrices by tandem dispersive liquid-liquid microextraction followed by high performance liquid chromatography.

作者信息

Asghari Alireza, Fahimi Ebrahim, Bazregar Mohammad, Rajabi Maryam, Boutorabi Leila

机构信息

Department of Chemistry, Semnan University, Semnan 2333383-193, Iran.

Department of Chemistry, Semnan University, Semnan 2333383-193, Iran.

出版信息

J Chromatogr B Analyt Technol Biomed Life Sci. 2017 May 1;1052:51-59. doi: 10.1016/j.jchromb.2017.03.012. Epub 2017 Mar 15.

Abstract

Simple and rapid determinations of some psychotropic drugs in some pharmaceutical wastewater and human plasma samples were successfully accomplished via the tandem dispersive liquid-liquid microextraction combined with high performance liquid chromatography-ultraviolet detection (TDLLME-HPLC-UV). TDLLME of the three psychotropic drugs clozapine, chlorpromazine, and thioridazine was easily performed through two consecutive dispersive liquid-liquid microextractions. By performing this convenient method, proper sample preconcentrations and clean-ups were achieved in just about 7min. In order to achieve the best extraction efficiency, the effective parameters involved were optimized. The optimal experimental conditions consisted of 100μL of CCl (as the extraction organic solvent), and the pH values of 13 and 2 for the donor and acceptor phases, respectively. Under these optimum experimental conditions, the proposed TDLLME-HPLC-UV technique provided a good linearity in the range of 5-3000ngmL for the three psychotropic drugs with the correlation of determinations (Rs) higher than 0.996. The limits of quantification (LOQs) and limits of detection (LODs) obtained were 5.0ngmL and 1.0-1.5ngmL, respectively. Also the proper enrichment factors (EFs) of 96, 99, and 88 for clozapine, chlorpromazine, and thioridazine, respectively, and good extraction repeatabilities (relative standard deviations below 9.3%, n=5) were obtained.

摘要

通过串联分散液液微萃取结合高效液相色谱 - 紫外检测(TDLLME - HPLC - UV),成功实现了对一些制药废水和人体血浆样品中某些精神药物的简单快速测定。通过连续两次分散液液微萃取,可轻松实现三种精神药物氯氮平、氯丙嗪和硫利达嗪的TDLLME。采用这种简便方法,仅需约7分钟即可实现适当的样品预浓缩和净化。为了获得最佳萃取效率,对相关有效参数进行了优化。最佳实验条件包括100μL的CCl(作为萃取有机溶剂),供体相和受体相的pH值分别为13和2。在这些最佳实验条件下,所提出的TDLLME - HPLC - UV技术对三种精神药物在5 - 3000ng/mL范围内具有良好的线性,测定相关系数(Rs)高于0.996。获得的定量限(LOQs)和检测限(LODs)分别为5.0ng/mL和1.0 - 1.5ng/mL。此外,氯氮平、氯丙嗪和硫利达嗪的富集因子(EFs)分别为96、99和88,萃取重复性良好(相对标准偏差低于9.3%,n = 5)。

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