超高效液相色谱串联质谱检测尿液中6种环境内分泌干扰物方法的建立与应用  

Establishment and Application of Ultra Performance Liquid Chromatography-Tandem Mass Spectrometry for Detecting Six Environmental Endocrine Disruptors in Urine

作　　者：彭凡立[1] 吉文亮[2] 彭丹红[3] 朱峰[2] 杨淼[1] 刘冉[1] 浦跃朴[1] 尹立红[1] 

机构地区：[1]东南大学公共卫生学院,环境医学工程教育部重点实验室,江苏南京210009 [2]江苏省疾病预防控制中心,江苏南京210009 [3]东南大学附属中大医院妇产科,江苏南京210009

出　　处：《环境与职业医学》2016年第5期499-503,共5页Journal of Environmental and Occupational Medicine

基　　金：国家自然科学基金(编号:81273123)

摘　　要：[目的]建立超高效液相色谱串联质谱（UPLC-MS/MS）检测人尿液中4种塑化剂代谢产物、双酚A（BPA）和壬基酚（NP）含量的方法,分析南京地区育龄期妇女对6种典型环境内分泌干扰物的暴露水平。[方法]建立针对塑化剂代谢产物、BPA和NP的尿液样品前处理方法以及UPLC-MS/MS检测方法,考察方法的回收率和日内、日间精密度。用所建立的方法对南京地区120份育龄期妇女尿液样品中塑化剂代谢产物、BPA和4-n-NP进行定量分析。[结果]4种塑化剂代谢产物、BPA和4-n-NP在1~100μg/L范围内均线性关系良好（r2〉0.998）,其中邻苯二甲酸单正丁酯（MBP）、邻苯二甲酸单异丁酯（Mi BP）、邻苯二甲酸单苄酯（MBz P）和邻苯二甲酸单（2-乙基）己酯（MEHP）检测限均为0.1μg/L。BPA和4-n-NP检测限为0.3μg/L。固相萃取回收率均在92.3%~103.5%,日间及日内精密度均小于10%。育龄期妇女尿液中MBP、Mi BP、MBz P、MEHP、BPA和4-n-NP质量浓度中位数分别为5.04、2.10、0.42、5.24、1.32和1.47μg/L。[结论]本研究建立的尿液中塑化剂代谢产物、BPA和4-n-NP检测方法具有灵敏度高、定量准确的优势。南京地区育龄期妇女尿液中MBP、Mi BP、MBz P、MEHP和BPA有较高检出率。[ Objective ] To establish a method based on ultra performance liquid chromatography-tandem mass spectrometry （UPLC-MS/MS） to assess six kinds of environmental endocrine disruptors including four phthalate metabolites （MPAEs）, bisphenol A （BPA）, and nonylphenol （NP） in the urine of women of reproductive age in Nanjing. [ Methods ] Pretreatment and UPLC- MS/MS analytical method was established for MPAEs, BPA, and NP. The accuracy, intra-day precision, and inter-day precision of the method were assessed. Then 120 urine samples collected from women of reproductive age in Nanjing were measured for concentrations of phthalate metabolites, BPA, and 4-n-NP. [ Results ] All the analytes were linear over the range of 1-100 μg/L （r2〉0.998）. The limits of detection were 0.1 μg/L for mono-n-butyl phthalate （MBP）, mono-isobutyl phthalate （MiBP）, mono-benzyl phthalate （MBzP）, and mono-2-ethylhexyl phthalate （MEHP）, and 0.3 μg/L for BPA and 4-n-NP. The recoveries by solid phase extraction of all analytes ranged from 92.3% to 103.5%; the intra-day and inter-day precisions were all less than 10%. The median concentrations of MBP, MiBP, MBzP, MEHP, BPA, and 4-n-NP were 5.04, 2.10, 0.42, 5.24, 1.32, and 1.47 μg/L, respectively. [ Conclusion ] The sensitive and accurate method is suitable for the determination of MPAEs, BPA and 4-n-NP in urine. Women of reproductive age present high positive rates of MBP, MiBP, MBzP, MEHP, and BPA.

关 键 词：塑化剂 双酚A 壬基酚 代谢产物 超高效液相色谱串联质谱 尿液 

分 类 号：R115[医药卫生—公共卫生与预防医学]