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研究了鳗鱼中醋酸甲羟孕酮的固相萃取-超高效液相色谱-串联质谱分析方法。样品用乙酸乙酯提取,经固相萃取柱净化后,40℃水浴氮气吹至近干;以乙腈和含有0.1%甲酸的水溶液为流动相,经ACQUITYTM UPLC BEH C18柱分离后进行超高效液相色谱-串联质谱多反应监测模式下的定性定量分析。醋酸甲羟孕酮检出限为0.03μg/kg、定量限为0.10μg/kg,添加量为0.10～5.0μg/kg时,醋酸甲羟孕酮在鳗鱼中的平均回收率大于80%,相对标准偏差小于10%。
Study on the solid phase extraction of medroxyprogesterone acetate in eel by ultra performance liquid chromatography-tandem mass spectrometry. The sample was extracted with ethyl acetate and purified by solid-phase extraction cartridge. The sample was blown to near dryness at 40 ° C in water bath. Acetonitrile and aqueous solution containing 0.1% formic acid were used as mobile phases and separated by ACQUITYTM UPLC BEH C18 column for ultra-high performance liquid chromatography Qualitative and Quantitative Analysis of Tandem Mass Spectrometry in Multiple Reaction Monitoring. The detection limit of medroxyprogesterone acetate was 0.03μg / kg, the limit of quantification was 0.10μg / kg, and the average recovery of medroxyprogesterone acetate in eels was more than 80% when the dosage was 0.10 ~ 5.0μg / kg, The standard deviation is less than 10%.