混合萃取剂-悬浮固化分散液相微萃取测定尿中的苯巯基尿酸  

Mixed Extractant-Dispersive Liquid Phase Microextraction Based on Solidification of Floating Organic Drop for Determination of S-phenylmercapturic Acid in Urine

作　　者：王宇[1] 邹晓莉[1] 张文滔 曾红燕[1] 张龙飞[1] 

机构地区：[1]四川大学华西公共卫生学院,成都610041 [2]成都市龙泉驿区疾病预防控制中心,成都610100

出　　处：《分析化学》2013年第5期749-753,共5页Chinese Journal of Analytical Chemistry

摘　　要：建立了混合萃取剂-悬浮固化分散液相微萃取联合高效液相色谱测定尿中苯巯基尿酸(S-phenylmer-capturic acid,SPMA)的方法。优化了微萃取的实验条件,取20 mL尿样并调节至pH 2.0,加入7.2 g固体NaCl,并振荡溶解;以100μL十二醇-三氯甲烷(1.8∶1,V/V)混合溶剂作为萃取剂,100μL甲醇作为分散剂,振摇使萃取剂分散于样液中;离心使萃取剂悬浮于样品溶液表面,"20℃冷冻至有机相凝固,转移凝固的萃取剂至EP管,室温下融化,离心后取上清液进样分析。苯巯基尿酸在0.025～1.25 mg/L浓度范围内线性良好,方法检出限为0.019 mg/L,日内精密度与日间精密度分别为2.2%～5.4%和2.5%～6.1%,将方法用于实际尿样的分析,取得了较满意的结果,加标回收率在86.8%～99.9%之间。本方法简便快捷、适合尿样批量分析。A method of dispersive liquid phase microextraction based on solidification of floating organic drop （SFO-DLLME） with mixed extractant by high performance liquid chromatography （HPLC） for the determination of S-phenylmercapturic acid （SPMA） in urine was established. Detailed research on the conditions of microextraction was evaluated in the experiment. An aliquot of 20 mL of urine sample was adjusted to pH 2.0 and 7.2 g NaCI was added to increase the ionic strength. Then, 100 ~L mixed solvent （ 1-dodecanol/chloroform, 1.8 ： 1, V/V） as extractant and 100 I^L methanol as dispersive agent were injected into sample solution. The solution was shaken to disperse the extractant. The extraction solvent could be floated on the surface of the solution with the help of centrifugation and solidified at -20 ~C. Then the solid organic phase was transferred to EP tube and melted at room temperature. The supernatant of mixed extraction solvent was injected into HPLC system for. The analytical method showed good linearity in the range of 0.025- 1.25 mg/L SPMA. The detection limit was 0. 019 mg/L. The intra-day and inter-day precisions （ relative standard deviation, RSD） of the method were 2.2% -5.4% and 2.5% -6.1% , respectively. The method was applied for determination of SPMA in human urine with satisfactory results. The spiked recoveries ranged from 86.8% -99.9%. The method was simple, fast and suitable for batch analysis of SPMA in urine samples.

关 键 词：混合萃取剂 悬浮固化分散液相微萃取 高效液相色谱法 苯巯基尿酸 尿样 

分 类 号：R446.12[医药卫生—诊断学] O658.2[医药卫生—临床医学]