水产品中多种雌激素残留的质谱分析方法研究

Mass Spectrometry Analysis of Diverse Estrogens in Aquatic Products

建立了同时测定7种雌激素残留的液相色谱一串联质谱法．在最优条件下，待测物呈现良好的线性关系，相关系数均大于0．9957，检测限介于0．5000—50．00ng／mL范围．鱼肉组织经C18小柱净化浓缩，4．0mL乙腈一水（体积比5：95，％）淋洗，2．0mL乙腈－水（体积比95：5，％）洗脱．三类鱼肉样品中（鲷鱼、龙胆鱼、多宝鱼）均检出双酚A和己二烯雌酚，部分样品中检出雌二醇和雌酮，加标回收率为85．70％～120．9％．方法快速、准确，适用于水产品中雌激素多残留的高效测定．

Simultaneous determination of seven estrogens residue was developed using liquid chromatography tandem mass spectrometry. Under the optimal conditions, target compounds presented good linear relationship with correlation coefficients larger than 0. 995 7 and limit of detections in the range of 0.500 0 - 50. 00 ng/mL. Fish tissue was extracted by a C18-solid phase extraction cartridge, washed with 4.0 mL of acetonitrile-H2O （5 ： 95, V/V, % ） , and then eluted with 2.0 mL of acetonitrile-H2O （95 ： 5, V/V, % ）. Both bisphenol A and dienestrol were detected in three different fish samples, while estradiol and estrone were detected in part of the samples. Recoveries were in the range of 85.70% - 120.9%. The proposed method is rapid, accurate and suitable to analyze diverse residue of estrogens in aquatic products.