脂肪酸基天然低共熔溶剂悬浮固化分散液-液微萃取/液相色谱法检测水样和人尿中抗真菌药

Determination of Antifungal Drugs in Water and Human Urine Samples by HPLC with Dispersive Liquid-Liquid Microextraction Based on Solidification of Floating Natural Containing Deep Eutectic Solvent Fatty Acid

建立了基于新制备的天然低共熔溶剂悬浮固化(SFNADES)分散液-液微萃取结合高效液相色谱法(HPLC)检测环境样品中酮康唑、克霉唑、特比萘芬和益康唑4种抗真菌药的分析方法。选用月桂酸为氢键供体,正辛醇为氢键受体合成的天然低共熔溶剂(NADES)作为萃取剂。通过优化萃取剂的种类与摩尔比、萃取剂体积、样品体积、样品pH值与离子强度、涡旋时间及离心时间等获得了最佳萃取效率。在最优条件下,方法的线性范围为0.56~500μg/L,线性系数(r^(2))≥0.999 8,检出限为0.17~0.80μg/L,定量下限为0.56~2.67μg/L,富集倍数为101~114,日内和日间相对标准偏差(n=6)分别不大于4.8%和5.4%。该方法已成功用于实际水样和人尿中抗真菌药的检测,回收率为91.5%~107%。

A high performance liquid chromatography(HPLC)with dispersive liquid-liquid micro⁃extraction was developed for the detection of antifungal drugs,including ketoconazole,clotrimazole,terbinafine and econazole in environmental samples,based on the solidification of floating natural deep eutectic solvent(SFNADES)wihic was newly synthesized with lauric acid as the hydrogen bond donor and 1-octanol as the hydrogen bond acceptor.The extraction conditions,including extractant type and molar ratio,extractant volume,sample volume,sample pH value,ionic strength,vortex time and centrifugation time were optimized to obtain the best extraction efficiency.Under the opti⁃mal conditions,the linear ranges of four antifungal drugs(r^(2)≥0.9998)ranged from 0.56μg/L to 500μg/L,with limits of detection(LODs)of 0.17-0.80μg/L,limits of quantitation(LOQs)of 0.56-2.67μg/L,and enrichment factors of 101-114.The intra-day and inter-day realtive stan⁃dard deviations(RSDs,n=6)were lower than 4.8%and 5.4%,respectively.The method was suc⁃cessfully applied to the detection of four antifungal drugs in real water and human urine samples with recoveries of 91.5%-107%.