液相色谱串联质谱法测定饲料中黄霉素A的含量

Ddetermination of FlavomycinA content in feed stuffs by Liquid chromatography tandem mass spectrometry

关键词:  液相色谱串联质谱  饲料  黄霉素A  测定

Key words:  Liquid chromatography tandem mass spectrometry  feed  FlavomycinA  determination

摘要:

建立了液相色谱―串联质谱法测定饲料中黄霉素A含量的检测方法，样品中的黄霉素A经氨水甲醇提取，HLB柱净化后，以Agilent Ecillps C18色谱柱为分析柱，乙腈-10 mM的乙酸铵为流动相进行梯度洗脱，经液相色谱―串联四级杆质谱多反应监测（MRM）模式下检测。该方法黄霉素A的线性范围为100～5000 μg/L，相关系数（r）为0.999725。依据S/N≥10确定方法的定量限为100 μg/kg。添加浓度在100～1000 μg/kg时，回收率在75%～95%之间，相对标准偏差（RSD）在4.7%～6.4%之间（n=5）。

Abstract:

To establish a liquid chromatography tandem mass spectrometry determination the content of Flavomycin A in feed, the FlavomycinA in sample extracted by ammonia methanol and purified by HLB column, Agilent Ecillps C18 chromatographic column as analysis column, Acetonitrile -10 mM ammonium acetate as gradient elution solution, then determined at multiple reaction monitoring( MRM) by liquid chromatography tandem mass spectrometry,The linear range of Flavomycin A was 100~ 5000 μg/L,correlation coefficient(r) was 0.999725. according S/N≥10 determination of the quantitation limit of Flavomycin A in the method is 100 μg/kg.when the additive concentration at the range of 100 ~ 1000 μg/kg, the mean recoveries ranging between 75% ~ 95%, and the relative standard deviations(RSD) between 4.7%～6.4%(n=5).