微波辅助酶解-超高效液相色谱串联质谱联用法快速检测尿液中的1-羟基芘  

Fast determination of 1-hydroxypyrene in human urine by microwave assisted enzymatic hydrolysis-ultra performance liquid chromatography-tandem mass spectrometry

作　　者：蒋举兴[1] 张敏[1,2] 王明锋[1] 者为[1] 段焰青[1] 王文元[1] 夏建军[1,2] 

机构地区：[1]红云红河烟草(集团)有限责任公司技术中心,云南昆明650202 [2]云南大学化学科学与工程学院,云南昆明650091

出　　处：《云南大学学报（自然科学版）》2014年第1期113-119,共7页Journal of Yunnan University(Natural Sciences Edition)

基　　金：云南中烟工业有限责任公司项目(2010JC11)

摘　　要：利用微波辅助酶解结合超高效液相色谱串联质谱联用法，建立了人体尿液中1-羟基芘的快速检测方法．通过对比酶解与碱解、恒温水浴酶解与微波辅助酶解、液液萃取与固相萃取等前处理方法对1-羟基芘检测的影响，最终采用微波辅助酶解、固相萃取作为样品检测的前处理方法．考察了基质效应，对比了纯溶剂与空白尿液配标准溶液2种不同的标准溶液配制方法，最终选用空白尿液来配制．方法的标准曲线方程为Y=1．24107x-0．130042，相关系数为0．9972，样品回收率在88．6％～97．1％之间，相对标准偏差在2．7％～12．6％之间．日内精密序为6．1％．日间精密序为6．2％．方洪榆涮阳为0．08ng／mL．宕J旨限为0．28ng/mL．A method for fast determination of I -hydroxypyrene （1 -OHP） in human urinary by microwave assisted enzymatic hydrolysis - ultra performance liquid chromatography - tandem mass spectrometry （ UPLC - MS/MS） was developed in this paper. The results of enzymatic hydrolysis compared with that of alkaline hydroly- sis, microwave assisted enzymatic hydrolysis compared with that of water bath enzymatic hydrolysis, and the liquid -liquid extraction compared with that of solid phase extraction were discussed, respectively. The preparation of standard solutions by blank urine and pure solvent were studied to reduce the matrix effect. Finally, the micro- wave assisted enzymatic hydrolysis and solid phase extraction were selected and the blank urine was used to pre- pare the standard solutions. The standard curve equation of the method was y = 1. 241 07x - 0. 130 042. The cor- relation coefficient was 0. 9972. The recovery was 88.6%---97.1%. The relative standard deviation was 2.7% to 12.6%. The intra - day precision was 6.1%. The inter - day precision was 6.2%. The detection limit was 0.08 ng/mL. The limit of quantification was 0.28 ng/mL. Compared with other existing methods, the established method in this paper for determination of urinary 1 - hydroxypyrene was more simple and accurate. Its efficiency, reproducibility and sensitivity were also satisfying.

关 键 词：1-羟基芘 液相色谱串联质谱 微波辅助 酶解 尿液 

分 类 号：O657.7[理学—分析化学] O625.1[理学—化学]