超声辅助离子液体分散液液微萃取/高效液相色谱法测定新型抗艾药ACC007

Determination of a Novel Anti-AIDS Drug ACC007 by High Performance Liquid Chromatography with Ultrasound-assisted Ionic Liquid Dispersive Liquid-Liquid Microextraction

该文提出了一种基于超声辅助离子液体分散液液微萃取/高效液相色谱(HPLC)测定血清及药片中ACC007含量的新方法。在超声辅助下,无需分散剂即可将疏水性离子液体1-辛基-3-甲基咪唑六氟磷酸盐([C8mimPF6])形成的细小液滴分散于样品溶液中,从而有效萃取ACC007,萃取率在94.0%以上。实验对萃取剂种类、萃取剂用量、溶液pH值、萃取时间、冷却和离心时间等萃取条件进行了考察。在优化条件下,ACC007的线性范围为0.20~10.0μg/mL,检出限分别为0.062μg/mL(药片)和0.068μg/mL(血清)。采用该方法对药片和血清中ACC007进行测定,加标回收率为90.5%~103%,相对标准偏差为2.9%~5.1%,结果令人满意。

In this paper,a simple and efficient method was developed and applied to the separation and determination of ACC007,a novel orally anti-AIDS drug in serum samples and its tablets,based on high performance liquid chromatography(HPLC)coupled with ultrasound-assisted ionic liquid dispersive liquid-liquid microextraction.The hydrophobic ionic liquid 1-octyl-3-methylimidazolium hexafluorophosphate([C8mimPF6])was used as extraction solvent.With the help of ultrasound,the ionic liquid could be divided into fine drops and dispersed entirely into sample solution without any dispersive solvent,promoting the analyte more easily migrating into the ionic liquid phase,and increasing the extraction rate up to 94.0%.Several important parameters affecting the extraction efficiency were investigated and optimized,including the type and volume of extraction solvent,pH value of sample,volume of sample,ultrasonication time,cooling time and centrifugation time.Under the optimized conditions,the calibration curves were linear over the range of 0.20-10.0μg/mL,with limits of detection(LOD)of 0.062μg/mL for tablet and 0.068μg/mL for serum,respectively.The proposed method was applied to the detection of human serum samples and ACC007 tablets with satisfactory results.The spiked recoveries ranged from 90.5%to 103%with relative standard deviations of 2.9%-5.1%.