摘要
建立了用凝胶渗透色谱-超高效液相色谱/串联三重四级杆质谱测定牛奶中黄曲霉毒素M_1的方法。方法以乙腈超声提取,凝胶渗透色谱净化后,以乙腈-0.1%甲酸（3：7,V/V）为流动相,UPLC BEH C18分离,ESI＋模式质谱检测,外标法定量。黄曲霉毒素M_1在0.1～4.0μg/L范围内线性关系良好,相关系数r为0.9955,检出限为0.01μg/kg,定量限为0.05μg/kg。牛奶样品在0.1,0.2,0.5μg/kg 3个加标浓度下,黄曲霉毒素M_1的回收率为72.4%～92.2%,相对标准偏差为4.0%～7.8%。
The method for determination of in milk and milk powder was developed using gel permeation chromatorgraphy（ GPC） coupled with ultra performance liquid chromatorgraphy-tandem mass spectrometry（ UPLC-MS /MS）.Sample was extracted with acetonitrile under ultrasonic operation and cleaned up with GPC.The fraction in 13 ～ 22 min was collected.The analyte was separated by UPLC BEH C18column（ 2.1 × 100 mm,1.7μm）using acetonitrile： 0.1% formic acid（ 3： 7,V/V） as mobile phase at the flow rate of 0.25 m L/min and detected under positive electrospray ionization（ ESI＋）,and quantified by the external standard method.The calibration curve was linear in the range of 0.1 ～ 4.0 μg/L with correlation coefficient of 0.9955.The limit of quantitation（ LOQ） was 0.05 μg /kg.Average recoveries of aflatoxin M_1 at three different spiked levels ranging from 72.4%to 92.2% with the relative standard deviations（ RSDs） from 4.0% to 7.8%.
出处
《分析试验室》
CAS
CSCD
北大核心
2016年第6期691-694,共4页
Chinese Journal of Analysis Laboratory
关键词
凝胶渗透色谱
超高效液相色谱-串联质谱仪
牛奶
奶粉
黄曲霉毒素M1
Gel permeation chromatorgraphy（GPC）
Ultra performance liquid chromatorgraphy-tandem mass spectrometry（UPLC-MS / MS）
Milk
Milk powder
Aflatoxin M1
