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尿样中两种三环类抗抑郁药丙咪嗪和曲米帕明经分散液液微萃取结合响应面优化后,用高效液相色谱法测定其超痕量。

High performance liquid chromatographic determination of ultra traces of two tricyclic antidepressant drugs imipramine and trimipramine in urine samples after their dispersive liquid-liquid microextraction coupled with response surface optimization.

作者信息

Shamsipur Mojtaba, Mirmohammadi Mehrosadat

机构信息

Department of Chemistry, Razi University, Kermanshah, Iran.

Department of Chemistry, Razi University, Kermanshah, Iran.

出版信息

J Pharm Biomed Anal. 2014 Nov;100:271-278. doi: 10.1016/j.jpba.2014.08.008. Epub 2014 Aug 13.

Abstract

Dispersive liquid-liquid microextraction (DLLME) coupled with high performance liquid chromatography by ultraviolet detection (HPLC-UV) as a fast and inexpensive technique was applied to the determination of imipramine and trimipramine in urine samples. Response surface methodology (RSM) was used for multivariate optimization of the effects of seven different parameters influencing the extraction efficiency of the proposed method. Under optimized experimental conditions, the enrichment factors and extraction recoveries were between 161.7-186.7 and 97-112%, respectively. The linear range and limit of detection for both analytes found to be 5-100ng mL(-1) and 0.6ng mL(-1), respectively. The relative standard deviations for 5ng mL(-1) of the drugs in urine samples were in the range of 5.1-6.1 (n=5). The developed method was successfully applied to real urine sample analyses.

摘要

分散液液微萃取(DLLME)结合高效液相色谱-紫外检测法(HPLC-UV)作为一种快速且经济的技术,被应用于尿液样本中丙咪嗪和三甲丙咪嗪的测定。响应面法(RSM)用于对影响该方法萃取效率的七个不同参数的效应进行多变量优化。在优化的实验条件下,富集因子和萃取回收率分别在161.7 - 186.7和97 - 112%之间。两种分析物的线性范围和检测限分别为5 - 100 ng mL⁻¹和0.6 ng mL⁻¹。尿液样本中5 ng mL⁻¹药物的相对标准偏差在5.1 - 6.1范围内(n = 5)。所建立的方法成功应用于实际尿液样本分析。

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