超高压液相色谱-串级质谱分析渔业水中7种激素药物

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ZORBAXSB-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0.5～40μggL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.

Determination of 7 hormones in fisheries water by ultra high-pressure liquid chromatography coupled tandem mass spectrometry

An ultra high-pressure liquid chromatography coupled electrospray ionization triple-qudruple tandem mass spectrometric(UHPLC-ESI MS/MS) method has been established for the simultaneous determination of 7 hormones,including cortisone acetate,cortisol,nandrolone prednisone,phenylpropionate,progesterone,Methyltestosterone and testosterone,in fisheries water.The hormones were extracted and cleaned up by an Oasis HLB solid phase extraction cartridge.The extract was evaporated to dryness under nitrogen,and reconstituted in acetonitrile-water(1:1,by volume).The 7 hormones were separated and detected by ZORBAX SB-C18(2.1×50 mm,1.8μm)using 0.1% formic acid(A) and acetonitrile(B) as mobile phase.The target compounds were confirmed and quantified by MS/MS under multiple reaction monitoring(MRM) mode with external standard method.Under the optimal conditions,the calibration curves of 7 hormones showed good linearity with the correlation coefficients >0.997 in the range of 0.5 or 1～40μg/L,the limits of detection(LODs) ranged from 0.03 to 0.3μg/L(S /N = 3),the average recoveries of 7 hormones were in the range 74.8%～113.0%,the relative standard deviations(RSDs) were 4.0%～16%.