固相萃取-高效液相色谱-串联质谱法同时测定尿液中16种羟基多环芳烃  

Determination of 16 kinds polycyclic aromatic hydrocarbons in urine by solid phase extraction combined with high performance liquid chromatography-tandem mass sepctrometry

作　　者：邹燕[1,2] 王顾希 李怀平[1,2] 冯德建 吴微[1,2] 王智 尹虹又[1,2] 李嘉骏 陈卿 曹佳[3] 叶善蓉 ZOU Yan;WANG Guxi;LI Huaiping;FENG Dejian;WU Wei;WANG Zhi;YIN Hongyou;LI Jiajun;CHEN Qing;CAO Jia;YE Shanrong(National Institute of Measurement and Testing Technology,Chengdu 610021,China;Standard and Testing Technology of Tea Key Laboratory of Sichuan Province,Chengdu 610021,China;Army Medical University,Chongqing 400038,China)

机构地区：[1]中国测试技术研究院,四川成都610021 [2]茶叶标准与检测技术四川省重点实验室,四川成都610021 [3]陆军军医大学,重庆400038

出　　处：《中国测试》2023年第11期119-126,共8页China Measurement & Test

基　　金：四川省重要技术标准研究项目(ZYBZ2022-23,ZYBZ2021-3)。

摘　　要：建立固相萃取-高效液相色谱-串联质谱法同时测定人体尿液中16种羟基多环芳烃(OH-PAHs)的含量。试样经过β-葡萄糖苷酸酶/硫酸酯酶酶解,HLB小柱富集净化,氮吹浓缩后0.1%维生素C乙腈溶液复溶,Agilent Eclipse PAH(2.1 mm×100 mm,1.8μm)分离,负离子多反应监测模式测定。各羟基多环芳烃线性范围良好,相关系数均>0.99,方法检出限范围为0.015~0.06 ng/mL,平均加标回收率范围为71.25%~114.07%。30份人体尿样检测结果显示2-OHNap、1-OHNap、2-OHFlu等10种均有检出,其检出率范围为23.33%~100%。该方法具有操作简便、灵敏度高、准确性好、适用性强、检测效率高、检测成本低等特点,可满足人体尿液中16种羟基多环芳烃含量的同时准确测定需要。A method was established for determination of 16 kinds polycyclic aromatic hydrocarbons(OH-PAHs)in urine by solid phase extraction combined with high performance liquid chromatography-tandem mass spectrometry(LC-MS/MS).Urine was hydrolyzed byβ-glucosidase/sulfate esterase,and purified by HLB solid phase extraction column,and redissolved by 0.1%vitamin C acetonitrile solution after nitrogen blowing and concentration,then separated on Agilent Eclipse PAH column(100 mm×2.1 mm,1.8μm)and detected in negative electrospray(ESI-)under multiple reaction monitoring(MRM)mode.OH-PAHs had good linearity(R>0.99),the limits of detection(LOD)was 0.015-0.06 ng/mL,the average recovery of OH-PAHs was 71.25%-114.07%.The results of 30 human urine samples showed that 10 kings polycyclic aromatic hydrocarbons including 2-OHNap,1-OHNap,and 2-OHFlu were detected,and the detection rates with a detection rate range of was 23.33%to 100%.The method is simple,high sensitivity,good accuracy,strong applicability,high detection efficiency and low detection cost.It can be used for the simultaneous determination of 16 kinds OHPAHs in urine.

关 键 词：人体尿液 固相萃取 羟基多环芳烃 高效液相色谱-串联质谱法 测定 

分 类 号：R446.1[医药卫生—诊断学] O657.63[医药卫生—临床医学] TB9[理学—分析化学]