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建立了同时测定渔业养殖水中氢化可的松、泼尼松、醋酸可的松、睾酮、甲睾酮、黄体酮及苯丙酸诺龙等7种激素残留药物的超高压液相色谱-电喷雾电离串联质谱(UPLC-ESI-MS/MS)分析方法。水样用HLB固相萃取柱净化、浓缩后,洗脱液经氮气吹干,残渣用乙腈-水(V:V=1:1)溶解,以乙腈和0.1%甲酸水溶液为流动相,经ZORBAX SB-C18色谱柱分离后进行LC-MS/MS多反应检测模式作定性定量分析。方法在0.5～40μg/L或1～40μg/L范围具有良好的线性,相关系数大于0.997,检出限(S/N=3)为0.03～0.3μg/L,平均回收率为74.8%～113.0%,相对标准偏差为4.0%～16%。方法适用于渔业养殖水中7种激素的检测分析。
A high pressure liquid chromatography-electrospray ionization (ESI-MS / MS) method was developed for the simultaneous determination of 7 hormones, including hydrocortisone, prednisone, cortisone acetate, testosterone, methyltestosterone, progesterone and nandrolone in fishery farming water Tandem mass spectrometry (UPLC-ESI-MS / MS) analysis method. The water sample was purified by HLB solid phase extraction (SPE) column. After concentration, the eluate was dried under nitrogen and the residue was dissolved in acetonitrile-water (V: V = 1: 1). Acetonitrile and 0.1% formic acid aqueous solution were used as mobile phases. After the separation of SB-C18 column, LC-MS / MS multiple reaction detection mode was used for qualitative and quantitative analysis. The method has a good linearity in the range of 0.5 ~ 40μg / L or 1 ~ 40μg / L, the correlation coefficient is greater than 0.997, the detection limit (S / N = 3) is 0.03 ~ 0.3μg / L and the average recovery is 74.8% ~ 113.0 %, Relative standard deviation of 4.0% to 16%. The method is suitable for the detection and analysis of seven hormones in fishery farming water.