固相萃取—微波衍生化—GC-MS法同时测定水中6种雌激素物质

建立了固相萃取—微波衍生化—气相色谱-质谱联用法快速同时测定水中雌酮（E1）、17α-雌二醇（α-E2）、17β-雌二醇（β-E2）、雌三醇（E3）、17α-乙炔基雌二醇（EE2）、双酚A（BPA）等6种雌激素物质的分析方法,对色谱柱升温程序、固相萃取及衍生化条件进行了优化。色谱柱最佳升温程序为：初始温度50 ℃,保持2 min;以20 ℃/min速率升至260 ℃,保持5 min;最后以10 ℃/min速率升至280 ℃,保持5 min。实验结果表明,在选取 HC-C18萃取小柱、添加双（三甲基硅烷基）三氟乙酰胺（BSTFA）+1%三甲基氯硅烷（TMCS）+吡啶作为衍生化试剂、微波315 W衍生化加热4 min的条件下,6种目标物标准曲线的相关系数均大于0.999,BPA、E1、EE2及E3的线性范围为3~300 ng/L,17α-E2及17β-E2的线性范围为5~300 ng/L,方法检出限为2.0~5.0 ng/L,加标回收率为76.45%~96.24%。

Simultaneous determination of six kinds of estrogens in water by SPE-microwave derivatization-GC-MS

A method for rapid and simultaneous determination of estrone（E1）,17α-estradiol （α-E2）,17β-estradiol（β-E2）,estriol（E3）,17α-ethynylestradiol（EE2）,and bisphenol A（BPA） in water by solid phase extraction（SPE）-microwave derivatization-gas chromatography-mass spectrometry was established. The heating procedure of chromatographic column and conditions for solid phase extraction and derivatization were optimized. The optimum heating programm of the column is as follows：initial temperature 50 ℃ for 2 min;heating to 260 ℃ at 20 ℃/min for 5 min;finally heating to 280 ℃ at 10 ℃/min for 5 min. The experimental results show that the 6 kinds of targets are selected under the conditions of using HC-C18 extraction cartridge,adding BSTFA+1% TMCS+pyridine as derivatization reagent and derivatization with 315 W microwave for 4 min. The correlation coefficients of the standard curves for the 6 kinds of targets are all greater than 0.999,the linear ranges are 3-300 ng/L for BPA,E1,EE2,E3 and 5-300 ng/L for 17α-E2 and 17β-E2. The detection limit of the method is 2.0-5.0 ng/L,and the standard recovery is 76.45%-96.24%..