超高效液相色谱-串联质谱法分析测定鱼肉中性激素多残留的研究

Simultaneous Determination of Sex Hormone in fish by UPLC-MS-MS

目的建立鱼肉中微量雄激素、孕激素和雌激素的超高效液相色谱串联质谱分析技术。方法以草鱼为代表,考察鱼肉中性激素在HLB固相萃取柱的提取净化效果,建立超高效液相色谱-串联质谱分析技术,在正/负电喷雾离子化多反应监测模式下分别测定雄激素、孕激素和雌激素。结果在最优条件下,鱼肉中14种性激素实现了快速、灵敏的分离检测,定量限(S/N≥10)为0.4～2μg·kg-1;应用于不同加标浓度的草鱼肉样品分析,回收率为60%～117%,RSD为6.7%～18.9%,符合国际公职分析化学家联合会(AOAC)要求。结论该方法检测灵敏度高,准确度和重现性好,在鱼肉中性激素多残留分析中效果良好。

OBJECTIVE To develop a method for the simultaneous determination of androgen, progesterone and estrogen in fish with ultra performance liquid chromatography-tandem mass spectrometry （UPLC-MS/MS）. METHODS Using Ctenopharyngodon idellus as the representative, the extraction and purification between sex hormones and HLB solid phase extraction column were investigated, and the method for sex hormone drugs has been established with UPLC-MS/MS. Under the positive or negative multi-reaction mode, sex homones including androgens, progesteronea and estrogens have been tested respectively. RESULTS Under the optimal conditions, fuorteen kinds of sex bormones in Ctenopharyngodon idellus were efficiently separated, and the limits of quantification （ LOQ, S/N≥10） were ranged from 0. 4 to 21μg·kg^-1. Appilied to the spiked samples,the average recoveries varied from 60% to 117% ,and the relative standard deviations （RSD） were between 6. 9% and 18.9%. These results could meet the level of AOAC. RESULTS CONCLUSION This method is sensitive, accurate and suitable for the simultaneous determination of hormones in fishs.