同位素稀释-液相色谱-串联质谱法测定动物源性食品中6种玉米赤霉醇类化合物

Determination of 6 zeranols residues in animal derived foods by liquid chromatography-tandem mass spectrometry with isotope dilution

目的建立动物源性食品中6种玉米赤霉醇类化合物残留量的同位素稀释-液相色谱-串联质谱的检测方法。方法样品加入同位素内标后,用甲醇提取,离心后上清液经50℃水浴氮气吹至近干,乙酸乙酯溶解残渣后,采用氨基小柱固相萃取,正己烷-乙酸乙酯（20∶80,V/V）和乙酸乙酯两种溶液洗脱后,氮气吹干,流动相溶解后,涡旋混匀过0.22μm有机滤膜后,LC-MS/MS多反应离子监测（MRM）模式检测,内标法定量。结果 6种玉米赤霉醇类化合物在3类动物源性食品中的加标回收率为84.8%-103.6%;RSD为3.7%-8.6%;检出限和定量限分别为0.03-0.07μg/kg和0.10-0.24μg/kg。结论该方法灵敏、准确,适用于动物源性食品中玉米赤霉醇类物质的检测。

Objective To establish a method for determination of 6 zeranols residues in animal derived foods by liquid chromatography-tandem mass spectrometry with isotope dilution. Methods The sample was added isotope internal standard and extracted using methanol. Methanol was nearly dried-up under nitrogen and the residue was dissolved with ethyl acetate. After solid phase extraction of amino cartridge,the eluent was dried-up by nitrogen at 50 ℃. The analytes were dissolved by the mobile phase and determined by liquid chromatography-tandem mass spectrometry. Results The recoveries of analytes were 84. 8%-103. 6%,and the relative standard deviations of detection were 3. 7%-8. 6%. The limits of detection and quantification were 0. 03-0. 07 μg / kg and 0. 10-0. 24 μg / kg. Conclusion The method is sensitive,accurate and it can meet the determination requirements of 6 zeranols residues in animal derived foods.