分析化学2009，Vol.37Issue(11)：1651-1656,6.
类固醇类环境内分泌干扰物羟基衍生化研究
Hydroxyl Group Derivatization of Steroid Environmental Endocrine Disrupting Chemicals
摘要
Abstract
The derivatization towards the hydroxyl groups of steroid environmental endocrine disrupting chemicals,such as estrone(E1),17β-estradiol(E2),estriol(E3) and 17α-ethynylestradoil( EE2),with A,O-bis (trimethylsilyl) trifluoroacetamide ( BSTFA ) as derivatization reagent followed by gas chromatography-mass spectrometry(GC-MS) was studied. The effects of the amount of BSTFA,derivatization temperature and time on the derivatization of target compounds,as well as the stability of steroid derivatives,calibration curves,instrumental quantification limits were investigated. The cleavage mechanism of steroid derivatives characteristic fragment ions was also interpreted. The results showed that better derivatization results were obtained when the amount of BSTFA was 25 μL for 100 μL steroids standard mix solution at 0.01 g/L;it is unnecessary to heating in the derivatization,better results were obtained when the steroids were derivatized with BSTFA at room temperature (20℃) for 10 min. The derivatives of target compounds were stable because their relative response factors(RRFs) had no observable change when deposited at -20℃ for 48 h. Under the optimal conditions,good linear correlation was obtained and the instrumental quantification limit was 0. 3μg/L for E1 and E2,while it was 5μg/L for EE2 and E3.关键词
气相色谱-质谱联用/类固醇/内分泌干扰物/羟基/衍生化/N,O-双三甲基硅基三氟乙酰胺Key words
Gas chromatography-mass spectrometry/steroid/endocrine disrupting chemicals/hydroxyl groups/derivatization/N/O-bis(trimethylsilyl)trifluoroacetamide分类
化学化工引用本文复制引用
黄斌,潘学军,刘晶靓,方锴,王宇,高建培..类固醇类环境内分泌干扰物羟基衍生化研究[J].分析化学,2009,37(11):1651-1656,6.基金项目
本文系国家自然科学基金(No.20767002),国家环保公益性行业科研专项基金(No.200809136),教育部留学回国人员科研启动基金(教外司留[2008]890号),云南省自然科学基金(No.2007B035M)及云南省教育厅重点基金(No.07Z11057)资助项目 （No.20767002）
