高效液相色谱-串联质谱法测定海水中雌酮、雌二醇、雌三醇

Determination of estrone,estriol,estradiol in seawater by liquid chromatography-tandem mass spectrometry

建立了测定海水中雌酮、雌二醇和雌三醇的高效液相色谱-串联质谱的分析方法。样品的提取方法为固相萃取,流动相为乙腈和0.1%氨水,梯度洗脱,流速0.2 mL/min,运行时间10 min。质谱采用负离子扫描模式,定量的碎片离子分别是：雌酮：269.02/144.99;雌二醇：271.04/182.96;雌三醇：287.03/170.94。仪器检出限均为0.001 ng,方法检出限均为0.2 ng/L。回收率分别是78.0-110.0%,82.2-103.2%,76.4-95.1%。该方法适用于海水中雌激素类物质的检测。

A method for the analysis of esrtone, estriol and estradiol was established. Samples were extracted by solidphase extraction instrument with a HLB columns, then determined by HPLC-Ms/Ms. The mobile phase was acetonitrile and 0.1% ammonia water, the flow rate was 0.2 mL/min, and running time was 10 min. The scan mode of mass spectrometry was negative ions, and fragment ions used for quantitative analysis were： estrone： 269.02/144.99, estriol： 271.04/182.96, estradiol： 287.03/180.94. Detection limits of these compounds were all 0.01 ng on a 10 μL of injection column, which allowed method detection limits of 2 ng/L. The recoveries of 3 estrogens were 78.0% 110.0%, 82.2% - 103.2%, 76.4% - 95.1% respectively. The results show that this method is applicable to estrogen monitoring in seawater.