液液萃取--超高效液相色谱串联质谱法同时测定尿中11种羟基多环芳烃  

Simultaneous determination of 11 hydroxy-polycyclic aromatic hydrocarbons in urine by LLE and UPLC-MS/MS

作　　者：谭磊[1] 邓芬芳[1] 卢祝靓子 罗晓燕[1] 潘心红[1] TAN Lei;DENG Fen-fang;LU Zhu-iang-zi;LUO Xiao-yan;PAN Xin-hong(Department of Toxicology and Biochemical Examination of Guangzhou Center for Disease Control and Prevention,Guangzhou 510440,China)

机构地区：[1]广州市疾病预防控制中心毒理与生化检验部,广州510440

出　　处：《环境卫生学杂志》2024年第1期72-78,共7页JOURNAL OF ENVIRONMENTAL HYGIENE

基　　金：广州市卫生健康科技项目(20221A011064)。

摘　　要：目的建立可同时测定尿中11种羟基多环芳烃(hydroxy-polycyclic aromatic hydrocarbons,OH-PAHs)的超高效液相色谱串联质谱分析(ultra-high performance liquid chromatography tandem with mass spectrometry,UPLC-MS/MS)法。方法尿液样品在pH=5.5条件下,在37℃水浴中经β-葡萄糖苷酸酶—芳基硫酸酯酶避光水解16 h,3.0 mL正己烷萃取、涡旋、离心,取上层有机相,重复萃取两次,合并萃取液,氮吹至近干,再复溶于20%乙腈水溶液中。流动相为水和10%异丙醇甲醇溶液,梯度洗脱模式洗脱,CORTECS C18色谱柱分离,ESI-模式测定尿液中11种羟基多环芳烃浓度,内标法定量分析。结果11种羟基多环芳烃线性关系良好,相关系数(r)均大于0.997。方法的检出限为0.01~0.10 ng/mL;日间回收率为79.8%~97.3%,精密度为1.9%~4.7%(n=3);日内回收率为78.6%~92.3%,精密度为3.7%~7.1%(n=3)。结论该方灵敏度高,准确可靠,适用于人群中多种羟基多环芳烃的监测。Objective To develop a method for simultaneous determination of 11 hydroxy-polycyclic aromatic hydrocarbons(OH-PAHs)in urine by ultra-high performance liquid chromatography tandem with mass spectrometry(UPLC-MS/MS).Methods The u-rine sample was hydrolyzed byβ-glucuronidase/arylsulfatase in a water bath at 37℃under the condition of pH 5.5 for 16 h away from light overnight,then extracted by 3.0 mL n-hexane.The upper organic phase was separated from urine sample by vortex and centrifu-gation.The extraction procedure was repeated twice and the two extracts were combined,and evaporated with nitrogen gas to almost dryness.The residues were re-dissolved in 20%acetonitrile solution,followed by gradient elution and separation by a CORTECS C18 column with 10%isopropanol methanol solution and water as mobile phases.The internal standard method was performed to measure the concentrations of 11 OH-PAHs by UPLC-MS/MS under ESI-mode.Results The method showed good linearity for the 11 OH-PAHs(r>0.997),with detection limits of 0.01-0.10 ng/mL.The inter-day recoveries were 79.8%-97.3%,with relative standard deviations of 1.9%-4.7%(n=3),and the intra-day recoveries were 78.6%-92.3%,with relative standard deviations of 3.7%-7.1%(n=3).Conclusion The proposed method is sensitive and accurate,and is suitable for the monitoring of multiple OH-PAHs in human urine samples.

关 键 词：超高效液相色谱串联质谱 羟基多环芳烃 液液萃取 尿液 

分 类 号：O657.6[理学—分析化学]