超声辅助悬浮固化液液微萃取-液相色谱荧光法测定血清中阿齐沙坦

Ultrasound-assisted Solidification of Floating Organic Drop Micro Extraction Coupled to High Performance Liquid Chromatography with Fluorescence Detection for the Determination of Azilsartan in Serum

建立一种悬浮固化分散液液微萃取-液相色谱荧光法测定血清中阿齐沙坦含量的新方法。在超声辅助下,乳化后的萃取剂1-十一醇高效快速萃取溶液中的阿齐沙坦,将萃取液离心后冰水浴中冷却,萃取剂凝固漂浮在水面而与溶液分离,分离后的1-十一醇用乙醇溶解后利用液相色谱荧光法测定其中阿齐沙坦的含量。实验中对液相色谱测定条件、萃取条件进行了优化,包括激发与发射波长、流动相组成、萃取剂用量、萃取溶液pH、超声时间、离心时间、冷却时间等。在优化条件下,工作曲线的线性范围为0.02~4.0μg/mL,最低检出限为6.0 ng/mL,回收率为93.1%~100.4%。专属性实验及血清样品测定结果表明该方法可以用于人血清中阿齐沙坦含量的测定。

This contribution reported a new method of ultrasound-assisted solidification of floating organic drop micro extraction coupled to high performance liquid chromatography with fluorescence detection(HPLC-FLD)for azilsartan in serum.Azilsartan could be extracted efficiently and rapidly into emulsified extractant 1-undecanol with the help of ultrasound technique.After centrifugation,the supernatant was cooled at ice bath,1-undecanol being solidified and floated on the water,which made 1-undecanol easily to be separated from aqueous solution.Finally,the azilsartan in 1-undecanol was dissolved in ethanol and measured by HPLC-FLD.The experiments were carried out to optimize the chromatographic and extraction conditions including excitation and emission wavelengths,composition of mobile phase,the volume of 1-undecanol,solution pH,ultrasonic time,centrifugation time,cooling time and etc.Under the optimal conditions,the calibration curve was linear over the range of 0.02~4.0μg/mL,and the limit of detection(LOD)was 6.0 ng/mL.The average recoveries range from 93.1%to 100.4%.The investigation indicates the established method could be used to determine azilsartan in human serum.