固相萃取-衍生化-气相色谱-质谱法测定水中类固醇类雌激素

GC-MS Determination of Steroid Estrogens in Water after Solid Phase Extraction Separation and Derivatization

采用固相萃取-衍生化-气相色谱-质谱法同时测定水中4种类固醇类雌激素雌酮(E1)、17β-雌二醇(E2)、17α-乙炔基雌二醇(EE2)、雌三醇(E3)。样品经Oasis HLB固相萃取柱,以丙酮为溶剂进行洗脱后,采用吡啶、N-甲基-N-三甲基硅基三氟乙酰胺于40℃衍生化20min后,采用气相色谱-质谱仪分析。E1、E2、EE2和E3的线性范围分别为5.00~500μg·L-1和10.0~500μg·L-1,4种类固醇类雌激素的检出限(3S/N)在1.5~3.0μg·L-1之间,测定下限(10S/N)在5.0~10μg·L-1之间;方法用于实际水样的分析,加标回收率在86.8%~93.8%之间,测定值的相对标准偏差(n=7)在7.1%~11%之间。

GC-MS with SPE separation and derivatization was applied to the simultaneous determination of estrone(E1),17β-estradiol(E2),17α-ethynylestradoil(EE2)and estriol(E3)in water.The sample was separated on Oasis HLB SPE column and the column was eluted with acetone.The eluate was derivatized with pyridine and NMethyl-N-(trimethylsilyl)trifluoroacetamide at 40 ℃for 20 min,and the derivates were then analyzed by GC-MS.The linearity ranges of E1,E2,EE2 and E3were 5.00-500μg·L-1 and 10.0-500μg·L-1,respectively.The detection limits(3S/N)and the limits of quantification(10S/N)were in the ranges of 1.5-3.0μg·L-1 and 5.0-10μg·L-1 respectively.Recovery found by standard addition method were in the range of 86.8%-93.8% and RSDs(n=7)found were in the range of 7.1%-11%.