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HPLC-MS/MS法同时测定食用油中黄曲霉毒素B1,B2,G1和G2

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采用高效液相色谱-串联质谱法测定食用油中黄曲霉毒素B1,B2,G1和G2.用甲醇-水溶液(70+30,V/V)将试样中的黄曲霉毒素B1,B2,G1和G2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B1,B2,G1和G2线性关系良好,线性相关系数均大于0.99,方法检出限为0.03 μg/kg时,响应值均大于3,方法定量限为0.1 μg/kg时,响应值均大于10.在1.0,5.0和8.0 μg/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.
Simultaneous Determination of Aflatoxins B1,B2,G1 and G2 in Edible Oil by HPLC-MS/MS
Determine aflatoxins B1,B2,G1,G2 in edible oil by High-performance liquid chromatography tandem mass spectrometry.This method extracts aflatoxins B1,B2,G,and G2 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 B1,B2,G1 and G2 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 0.03 μg/kg,the response values of all three compounds were greater than 3.When the limit of quantification of the method was 0.1 μg/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 8.0 μg/kg,and the relative standard deviations were 1.24%-5.56%(n=7).The results meet the requirement of method verification.

high performance liquid chromatography-tandem mass spectrometryedible oilaflatoxins

双杨、夏林林、赵燕、吴磊磊、陈银华、段少奇

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十堰市食品药品检验检测所(十堰 442000)

十堰市黄龙镇中心小学(十堰 442000)

高效液相色谱-串联质谱法 食用油 黄曲霉毒素

2024

食品工业
上海市食品工业研究所

食品工业

影响因子:0.47
ISSN:1004-471X
年,卷(期):2024.45(8)