UPLC-MS/MS法测定牛乳中己烯雌酚、玉米赤霉醇和玉米赤霉酮残留

Determination of diethylstilbestrol, zearanol and zearelone residues in milk by UPLC-MS/MS method

建立了牛乳中己烯雌酚、玉米赤霉醇和玉米赤霉酮的超高效液相色谱-串联质谱（UPLC-Ms／Ms）快速检测法。牛乳中的目标物经乙腈提取后，在上清液中加入一定比例的水，并调节pH值至11.0，再经MAX固相萃取柱净化、浓缩，超高效液相色谱-串联质谱仪测定，外标法定量。方法中己烯雌酚、玉米赤霉醇和玉米赤霉酮的回收率分别为72.3％-94.5％、72.8％-87.4％和88.9％-110.6％。该方法快速、准确，回收率高，可用于牛乳中己烯雌酚、玉米赤霉醇和玉米赤霉酮的快速检测。

The paper establishes a method to determine diethylstilbestrol, zearanol and zearelone contents in milk using UPLC-MS/MS. Ace-tonitrile was added to milk samples to extract target ingredient, add some water into the supernatant and adjust pH value to 11.0, and then concentrated by MAX SPE procedureapp：ds：successively. Diethylstilbestrol, zearanol and zearelone contents were measured by UPLC-MS/MS. The recoveries of diethylstilbestrol, zearanol and zearelone are 72.3%-94.5%、 72.8%-87.4% and 88.9% - 110.6% respectively, shows that the method is meet the demand to determine diethylstilbestrol, zearanol and zearelone contents in milk.