亲水作用色谱-串联质谱法测定职业暴露人群尿中芳香烃代谢产物  

Hydrophilic interaction chromatography-tandem mass spectrometry for determination of aromatic hydrocarbon metabolites in urine samples of occupationally exposed population

作　　者：任建伟 朱婧[1] 罗新月 赵璇 杨觅 赵心悦 张静[1] 邹晓莉[1] REN Jian-wei;ZHU Jing;LUO Xin-yue;ZHAO Xuan;YANG mi;ZHAO Xin-yue;ZHANG Jing;ZU Xiao-Li(Department of Laboratory Technology and Science of Public Health,West China School of Public Heath and West China Fourth Hospital,Sichuan Unicersity,Chengdu,Chengdu 610041,China)

机构地区：[1]四川大学华西公共卫生学院/四川大学华西第四医院卫生检验与检疫系,成都610041

出　　处：《现代预防医学》2021年第3期515-519,共5页Modern Preventive Medicine

基　　金：四川省卫生和计划生育委员会重点研究项目(17ZD048);四川省科学技术厅重点研发项目(2020YFS0056)。

摘　　要：目的建立直接稀释-亲水作用色谱-串联质谱法同时测定尿中芳香烃代谢产物的方法。方法尿样经酶解后,用含同位素内标的甲酸铵溶液稀释10倍,过滤后用于分析。色谱分离采用ACQUITY UPLC~?BE H HILIC色谱柱(50 mm×3 mm,1.7μm),流动相采用5 mmol/L甲酸铵和乙腈,梯度洗脱。质谱采用电喷雾电离源、正负离子交替扫描模式和多反应监测模式进行检测,内标标准曲线定量。结果各目标化合物线性良好,检出限在0.33~6.18μg/L之间,定量限在1.10~20.6μg/L之间。加标回收率为89.3%~107%,日内和日间精密度分别为0.72%~7.07%和1.58%~10.6%。结论建立的方法快速灵敏,可满足职业健康体检的需求。职业暴露人群尿样分析显示,某些生产企业和岗位有一定的暴露风险,须加强监管、完善个人防护。Objective To establish a direct dilution-hydrophilic interaction chromatography-tandem mass spectrometry method for the simultaneous determination of aromatic hydrocarbon metabolites in urine samples. Methods Urine samples were enzymatically digested and the enzymatic hydrolysate was diluted 10 times with ammonium formate containing isotope internal standards. After being filtered, the supernatant was used for analysis. ACQUITY UPLC○CBEH HILIC hydrophilic interaction chromatography column(50 mm×3 mm, 1.7 μm) was adopted for the chromatographic separation, and 5 mmol/L ammonium formate and acetonitrile were employed as the mobile phases for gradient elution. Electrospray ionization source(ESI) was adopted for mass spectrometric detection with positive and negative ion alternate scanning mode and multiple reaction monitoring mode, and the internal standard calibration curve for quantification. Results Each target compound had good linearity, the detection limits were between 0.33-6.18 μg/L, and the quantification limits were between 1.10-20.6 μg/L. The spiked recovery rates of the method were 89.3%-107%, and the intra-day and inter-day precisions were 0.72%-7.07% and 1.58%-10.6%, respectively. Conclusion The established method is fast and sensitive and it meets the requirements of occupational health examinations. The analysis results of urine samples of occupationally exposed population showed that there are certain exposure risks in some production companies and positions. It is suggested that the supervision of occupational places should be strengthened to improve personal protection.

关 键 词：芳香烃 同位素稀释法 亲水作用色谱-串联质谱法 职业暴露 

分 类 号：R115[医药卫生—公共卫生与预防医学]