| 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。 |
| 关键词: 牛奶 激素类药物 超高效液相色谱-串联质谱法 |
| DOI： |
| 投稿时间：2021-03-16修订日期：2021-07-07 |
| 基金项目:宁夏回族自治区重点研发计划重大 (重点) 项目“畜禽产品质量安全评估与监控技术应用研究” (2018BBF02002) |
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| Determination of 11 Hormones Residues in Milk Using QuEChERS by Ultrahigh-performance Liquid Chromatography-tandem Mass Spectrometry |
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| (Ningxia Institute of Veterinary and Feed) |
| 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. |
| Key words: milk hormones Ultrahigh-performance Liquid Chromatography-tandem Mass |
