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.
作者
邹燕
王顾希
李怀平
冯德建
吴微
王智
尹虹又
李嘉骏
陈卿
曹佳
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)
出处
《中国测试》
CAS
北大核心
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)。
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
urine
solid phase extraction
polycyclic aromatic hydrocarbons(OH-PAHs)
high performance liquid chromatography-tandem mass spectrometry(LC-MS/MS)
determination
