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1.0μg/kg;牛奶样品中11种激素类药物在1.0~10μg/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。
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 1.0μg/kg.The average recoveries of 11 hormones in milk samples were between 60.3%~119.6%at the addition level of 1.0~10μg/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.
作者
陈娟
李永琴
卜宁霞
马岩
杨奇
CHEN Juan;LI Yong-qing;BU Ning-xia;MA Yan;YANG Qi(Ningxia Supervision Institue for Veterinary Drugs and Administration,Ningxia,Ying chuan,750011,China)
出处
《中国兽药杂志》
2021年第8期27-33,共7页
Chinese Journal of Veterinary Drug
基金
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)。
