气相色谱—质谱分析5种雌激素类物质的衍生化方法优化  

Optimization of derivatization for the analysis of five kinds of estrogens by GC-MS

作　　者：王欣 顾弘理 沈剑[1] 仝欣楠[1] 王欣泽[1] WANG Xin;GU Hongli;SHEN Jian;TONG Xinnan;WANG Xinze(School of Environmental Science and Engineering,Shanghai Jiao Tong University,Shanghai 201100)

机构地区：[1]上海交通大学环境科学与工程学院,上海201100

出　　处：《环境污染与防治》2018年第8期890-895,共6页Environmental Pollution & Control

基　　金：国家水体污染控制与治理科技重大专项(No.2012ZX07105-003)

摘　　要：选取5种雌激素类物质雌酮(E1)、雌二醇(E2)、17α-雌二醇(EE2)、雌三醇(E3)、双酚A(BPA)为研究对象,在气相色谱(GC)—质谱(MS)联用分析方法的基础上,对衍生化试剂和衍生化反应条件进行了优化。结果表明,使用含有1%(质量分数)三甲基氯硅烷(TMCS)的N,O-双(三甲基甲硅烷基)-三氟乙酰胺(BSTFA)联合吡啶作为衍生化试剂,加热条件为烘箱70℃加热40min时,衍生化产物单一且灵敏度高。采用此优化方法得到5种物质的平均加标回收率为98.0%~104.3%,相对标准偏差(RSD)为0.4%~12.5%,可为环境中5种雌激素类物质的分析测定提供参考。An optimized derivatization method for the simultaneous determination of five kinds of estrogens estrone,estradiol,estriol,ethinyl estradiol and bisphenol A by GC-MS was developed in this study.The combined use of N,O-bis(trimethylsilyl)-trifluoroacetamide(BSTFA)with 1%(mass fraction)trimethylchlorosilane(TMCS)and pyridine as derivatization reagent,together with 40 min heating in the oven at 70℃,was found to be the most efficient method for stable derivatives and high sensitivity.The method exhibited good accuracy(recoveries of 98.0%-104.3%)and precision(relative standard deviations of 0.4%-12.5%),which could provide reference for the subsequent analysis of five kinds of estrogens.

关 键 词：雌激素 衍生化 烘箱加热 气相色谱-质谱 

分 类 号：X832[环境科学与工程—环境工程]