QuEChERS-超高效液相色谱-串联质谱法检测牛奶中11种激素类药物残留

Determination of 11 Hormones Residues in Milk Using QuEChERS by Ultrahigh-performance Liquid Chromatography-tandem Mass Spectrometry

关键词:  牛奶  激素类药物  超高效液相色谱-串联质谱法

Key words:  milk  hormones  Ultrahigh-performance Liquid Chromatography-tandem Mass

摘要:

建立超高效液相色谱-串联质谱法(UPLC-MS/MS)测定牛奶中11种激素类药物残留的检测方法。样品经乙酸乙酯提取，氮气吹干，残留物用0.1 %甲酸50 %乙腈水溶液溶解后，经Cleaner MAS-Q 净化管净化，滤膜过滤后用超高效液相色谱-串联质谱仪测定，基质外标法定量。在0.5～100 ng/mL的浓度范围内11中激素类药物峰面积与浓度呈良好的线性相关，相关系数均大于0.998；方法的定量限为1.0 μg/kg；牛奶样品中11种激素类药物在1.0～10 μg/kg添加水平内的平均回收率在60.3 %～119.6 % 之间，批内、批间相对标准偏差在0.2 %～12.1 %之间。该方法灵敏、准确、重现性良好，能够满足残留检测要求。

Abstract:

A method for determination of 11 hormones residues in milk by Ultrahigh-performance liquild chromatography-tandem mass spectrometry was established. Samples were extracted with acetomitrile and then dried through nitrogen.The residues were dissolved with 50 % acetonitrile water (containing 0.1 % formic acid) and then purified by Cleaner MAS-Q, filtered with membrane and determined by ultrahigh-performance liquild chromatography mass spectrometer. In the concentration range of 0.5～100 ng/mL,the peak areas of 11 hormones showed a good linear correlation with the concentration,and the correlation were all higher than 0.998.The detection limit of the method was 1.0 μg/kg.The average recoveries of 11 hormones in milk samples were between 60.3 %～119.6 % at the addition level of 1.0～10 μg/kg. The relative standard deviation (RSD) was between 0.2 %～12.1 %. The method is sensitive, accurate and reproducible, which can meet the requirements of residue detection.