摘要
采用高效液相色谱-串联质谱法测定食用油中黄曲霉毒素B_(1),B_(2),G_(1)和G_(2)。用甲醇-水溶液(70+30, V/V)将试样中的黄曲霉毒素B_(1),B_(2),G_(1)和G_(2)进行提取,提取液用含1%吐温-20的PBS溶液稀释后,通过免疫亲和柱净化和富集,净化液浓缩、定容和过滤后经液相色谱分离,串联质谱检测,同位素内标法定量。结果显示,在0.1~10.0 ng/mL质量浓度范围内黄曲霉毒素B_(1),B_(2),G_(1)和G_(2)线性关系良好,线性相关系数均大于0.99,方法检出限为0.03μg/kg时,响应值均大于3,方法定量限为0.1μg/kg时,响应值均大于10。在1.0, 5.0和8.0μg/kg浓度水平上加标回收率为73.0%~105.0%,相对标准偏差(n=7)为1.24%~5.56%,满足方法验证要求。
Determine aflatoxins B_(1),B_(2),G_(1),G_(2) in edible oil by High-performance liquid chromatography tandem mass spectrometry.This method extracts aflatoxins B_(1),B_(2),G_(1) and G_(2) from the sample by methanol water solution(70+30,V/V),the extraction solution was diluted with PBS solution containing 1%Tween-20,purified and enriched through an immunoaffinity column.After concentration,constant volume and filtration of the purified liquid,it was separated by liquid chromatography,detected by tandem mass spectrometry and quantified by isotope internal standard method.The results showed that the linear relationship among the aflatoxins B_(1),B_(2),G_(1) and G_(2) was good in the concentration range of 0.1-10.0 ng/mL.The linear correlation coefficients were greater than 0.99.When the detection limit of the method was 0.03μg/kg,the response values of all three compounds were greater than 3.When the limit of quantification of the method was 0.1μg/kg,the response values of all three compounds were greater than 10.The recoveries were 73.0%-105.0%at the concentrations of 1.0,5.0 and 8.0μg/kg,and the relative standard deviations were 1.24%-5.56%(n=7).The results meet the requirement of method verification.
作者
双杨
夏林林
赵燕
吴磊磊
陈银华
段少奇
SHUANG Yang;XIA Linlin;ZHAO Yan;WU Leilei;CHEN Yinhua;DUAN Shaoqi(Shiyan Institute for Food and Drug Control,Shiyan 442000;Central Primary School of the Huanglong Town,Shiyan 442000)
出处
《食品工业》
CAS
2024年第8期299-303,共5页
The Food Industry
关键词
高效液相色谱-串联质谱法
食用油
黄曲霉毒素
high performance liquid chromatography-tandem mass spectrometry
edible oil
aflatoxins
