超高效液相色谱-串联质谱法测定鳗鱼中醋酸甲羟孕酮含量

Determination of medroxyprogesterone acetate residues in eels by ultra performance liquid chromatography with tandem mass spectrometric detection

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%。

The solid phase extraction-ultra performance liquid chromatography with electrospray ionization tandem mass spectrometry（UPLC-ESI-MS/MS） method for determination of medroxyprogesterone acetate in eels has been established in our work.The drugs were extracted by ethyl acetate,and then on the solid phase extraction cartridges,and the extraction was evaporated at 40 ℃ by nitrogen blow.The residue was dissolved and separated by ACQUITYTM UPLC BEH C18 column,and mobile phase was A（acetonitrile） and B（0.1% formic acid in water） and finally was confirmed and quantified using a MS/MS system in the multiple reaction mode with tandem mass analyzer using positive polarity mode.The LOD of medroxyprogesterone acetate was 0.03 μg/kg,and the LOQ was 0.10 μg/kg,and the average recovery was more than 80% with spiked residues from 0.10 μg/kg to 5.0 μg/kg.The intra-day relative standard derivation（RSD） and the inter-day RSD were less than 10%.The method has merits of simplicity,sensitivity and rapidity,and it can be used for determination in eels.