ASE净化-HPLC-MS/MS法测定动物源性食品中12种多肽类抗生素  

Determination of 12 Kinds of Polypeptide Antibiotics in Animal Derived Food by ASE with HPLC-MS/MS

作　　者：黄孟丽 张博文 江改青 胡文彦 刘真 HUANG Mengli;ZHANG Bowen;JIANG Gaiqing;HU Wenyan;LIU Zhen(Nanjing Institute for Food and Drug Control,Nanjing 210038,China)

机构地区：[1]南京市食品药品监督检验院,江苏南京210038

出　　处：《食品科技》2023年第5期278-286,共9页Food Science and Technology

基　　金：国家市场监督管理总局科技计划项目(2020MK140)。

摘　　要：目的:建立加速溶剂萃取(ASE)净化-液相色谱-串联质谱联用仪(HPLC-MS/MS)同时测定动物源性食品中12种多肽类抗生素的方法。方法:样品称取2.0 g经ASE进行前处理,采用Phenomenex色谱柱分离,以0.1%甲酸乙腈溶液和0.1%甲酸水溶液为流动相进行梯度洗脱,质谱采用电喷雾正离子多反应模式。结果:12种多肽类物质在4.0~50.0 ng/mL时线性关系良好(R2>0.99),定量限为0.05~0.5 mg/kg,在猪肉和鱼肉基质中0.1、0.3、1 mg/kg 3个添加水平下回收率为71.0%~119.8%,相对标准偏差为2.3%~14.9%(n=6)。结论:该方法简单、快速、高效,适用于动物源性食品中12种多肽类抗生素的测定。Objective:A method for the simultaneous determination of 12 polypeptide antibiotics in animal derived food by accelerated solvent extraction(ASE) combined with liquid chromatography-tandem mass spectrometry(HPLC-MS/MS) was established.Methods:2.0 g samples were pretreated with ASE,and then the target analytes were separated on a Phenomenex column using a gradient elution of 0.1% formic acid acetonitrile solution and 0.1% formic acid water solution.Positive ion of electrospray ionization(ESI)and multiple reaction monitoring(MRM) mode were used for detection.Results:Good linear relationships of the 12 polypeptide antibiotics were obtained,and the correlation coefficients were all greater than 0.99within the concentration range of 4.0-50.0 ng/mL.The limits of detection(LOD) were range of 0.05 mg/kg to 0.5 mg/kg.The recovery experiments were performed with pork and fish,the mean recoveries varied from 71.0% to 119.8% at three spiked levels(0.1,0.3,1 mg/kg),and the relative standard deviations ranged from 2.3% to 14.9%(n=6).Conclusions:The method is simple,rapid and efficient,and is suitable for the simultaneous determination of 12 polypeptide antibiotics in animal derived food.

关 键 词：加速溶剂萃取(ASE) 液相色谱-串联质谱(HPLC-MS/MS) 多肽类抗生素 

分 类 号：TS207.5[轻工技术与工程—食品科学]