建立了乳制品中5种激素残留的液相色谱-串联质谱快速测定方法.固体样品用水溶解后加甲醇提取（液体样品直接加甲醇提取）,提取液经CNWBOND LC-C18固相萃取柱净化后,采用ZORBAX SB-C18色谱柱（100×2.1mm,3.5μm）分离,分别在电喷雾正、负离子模式下以多反应监测模式检测待测组分.正离子模式下的流动相为乙腈-0.1%甲酸（V/V）水溶液,负离子模式下的流动相为乙腈-5mmol/L乙酸铵溶液.在该优化条件下,5种激素在相应的浓度范围内相关系数均大于0.99,方法回收率为77.2%~89.6%,相对标准偏差为3.91%~8.49%,定量限（LOQ,S/N≥10）为1~20μg/kg.
Abstract：A quick method for determining the residues of 5 hormones in dairy by liquid chromatography- tandem mass spectrometry was developed. Solid sample was dissolved in water, then extracted with methanol （liquid sample was extracted by methanol directly）. The purification was carried out on C18 solid phase extraction column and separation was performed using a ZORBAX SB-C18 column by gradient elution. Electrospray ionization mass spectrometry was operated in the positive or negative multi-reaction monitoring mode for the analytes. Acetonitrile and water with 0. 1% （V/V） formic acid were used as mobile phase in the positive mode. Acetonitrile and water with 5 mmol/L ammonium acetate were used as mobile phase in the negative mode. Under the optimized conditions, the correlation coefficients of linear calibration curves were over 0. 99 in the corresponding concentration range. The overall recoveries varied from 77.2% to 89.6% ,and the relative standard deviations were from 3.91% to 8.49 %. The limits of quantifieation（LOQ,S/N= 10） were from 1 μg/kg to 20 μg/kg.
Journal of Analytical Science
Liquid chromatography-tandem mass spectrometry
Solid phase extraction