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

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

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%。

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%..