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固相萃取结合分散液液微萃取/高效液相色谱-紫外法作为一种灵敏、高效的方法,用于提取、预浓缩和同时测定药物制剂和生物样品中的抗逆转录病毒药物奈韦拉平、依非韦伦和奈韦拉平。

Solid-phase extraction combined with dispersive liquid-liquid microextraction/HPLC-UV as a sensitive and efficient method for extraction, pre-concentration and simultaneous determination of antiretroviral drugs nevirapine, efavirenz and nelfinavir in pharmaceutical formulations and biological samples.

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. 2019 Mar 20;166:95-104. doi: 10.1016/j.jpba.2019.01.003. Epub 2019 Jan 4.

DOI:10.1016/j.jpba.2019.01.003
PMID:30639934
Abstract

Therapeutic drug monitoring (TDM) of antiretroviral drugs requires accurate and precise analysis of their trace amounts in plasma samples. Solid-phase extraction (SPE) coupled with dispersive liquid-liquid microextraction based on solidification of floating organic drop (DLLME-SFO) was introduced as a simple and sensitive method for extraction, pre-concentration and simultaneous determination of efavirenz (EFV), nelfinavir (NFV) and nevirapine (NVP) in human plasma and pharmaceutical formulations by using high performance liquid chromatography (HPLC) with UV detection. A response surface methodology (RSM) based on central composite design (CCD) was used for optimizing the main variables in the extraction procedure. Under the optimum experimental conditions, the calibration curves were linear in the range of 0.1-400 ng mL with correlation coefficients from 0.9982 to 0.9997 and limits of detection (at S/N = 3) of 0.03 to 0.07 ng mL. Moreover the intra-day and inter-day precision (RSD%) were in the range of 2.2-4.2% and 3.1-5.2%, respectively. The enrichment factors and relative recoveries of the anti-HIV drugs were 459-1507 and 93.7-105.4%. The method was successfully applied to the simultaneous determination of the trace amounts of the antiretroviral drugs in blood plasma and pharmaceutical formulations.

摘要

治疗药物监测(TDM)需要准确、精确地分析血浆样本中痕量的抗逆转录病毒药物。固相萃取(SPE)与基于悬浮有机液滴固化的分散液相微萃取(DLLME-SFO)相结合,被引入作为一种简单灵敏的方法,用于通过高效液相色谱法(HPLC)与紫外检测,提取、预浓缩和同时测定人血浆和药物制剂中的依非韦伦(EFV)、奈韦拉平(NFV)和奈韦拉平(NVP)。响应面法(RSM)基于中心复合设计(CCD)用于优化萃取过程中的主要变量。在最佳实验条件下,校准曲线在 0.1-400ng/mL 范围内呈线性,相关系数为 0.9982 至 0.9997,检测限(S/N=3)为 0.03 至 0.07ng/mL。此外,日内和日间精密度(RSD%)分别在 2.2-4.2%和 3.1-5.2%范围内。抗 HIV 药物的富集因子和相对回收率分别为 459-1507 和 93.7-105.4%。该方法成功应用于同时测定血浆和药物制剂中痕量抗逆转录病毒药物。

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