SPE-UPLC-Q-TOF/MS测定水环境中的雌激素

Determination of Estrogens in Water Samples by SPEUPLC-Q-TOF /MS

研究建立了固相萃取、超高效液相色谱-四极杆串联飞行时间质谱（UPLC-Q—TOF／MS）测定水环境中6种雌激素（雌三醇、雌二醇、炔雌醇、雌酮、己烯雌酚、双酚A）的分析方法。水样经甲醇活化后的C18固相萃取小柱富集浓缩，用10mL10％的甲醇溶液淋洗，10mL纯甲醇洗脱，洗脱液经高纯氮气吹至0．4mL后用UPLC-Q-TOF／MS测定。6种常见的雌激素质量浓度在0．5—100μg／L范围内时，具有良好的线性（R〉0．9937），检出限介于5．60—10．6ng／L之间。空白加标水样为1μg／L的水平下，相对标准偏差（RSD）为2．8％-9．0％，其加标回收率为75％-101％。该方法可用于水体中雌激素的分析测定。

A solid phase extraction （ SPE ） -ultra-performance liquid chromatography coupled to quadrupole time-of-flight mass spectrometry （UPLC-Q-TOF/MS） method was estab- lished for the simultaneous determination of six estrogens （estriol, estradiol, 17a-ethinylestradiol, estrone, diethylstilbestrol and bisphenol A） in water. The compounds in 1 000 mL water sample were extracted by C18 column,washed by 10% methanol（ volume percentage） , eluted by the 10 mL methanol, The eluent was blowed to 0.4 mL by nitrogen and then analyzed qualitatively and quantitatively by UPLC-Q-TOF/MS. Six fro-quent estrogens had good linearity in the range of 0. 5 × 100 μg/L（R 〉0. 993 7） with the limits of detection（LODs） ranging from 5.60 to 10. 6 ng/L. At the levels of 1 μg/L,the relative standard deviations between 2.8% and 9.0 % with the average recoveries ranged from 75% to101%. The method can be used for the determination of estrogen in water environment.