超高压液相色谱-串联质谱法测定食用植物油中4种黄曲霉毒素B1、B2、G1、G2
目的 建立测定食用植物油中黄曲霉毒素B1、B2、G1、G2的优质高效的分析方法。方法 采用超高压液相色谱-串联质谱(UPLC-MS/MS)法。样品用乙酸乙酯提取, 弗罗里硅土小柱净化, 经 C18色谱柱分离, 以电喷雾离子源在正离子多反应监测(MRM)模式下进行测定, 外标法定量。结果 黄曲霉毒素B1、B2、G1、G2的检出限均为0.04 ?g/kg, 定量限均为0.10 ?g/kg, 在0.1~20 ?g/L范围内线性关系良好, 相关系数r分别为0.9986, 0.9986, 0.9992, 0.9996。在0.1~5.0 ?g/kg加标水平内黄曲霉毒素B1、B2、G1、G2的回收率为79.1%~94.6%, RSD为5.0 %~9.6%。结论 该方法实用、准确、灵敏, 适用于食用植物油中黄曲霉毒素残留量的测定。
Objective To establish a high-quality and efficiency method for the determination of aflatoxin B1、B2、G1、G2 in edible vegetable oil. Methods The ultra-pressure liquid chromatography-tandem mass spec-trometry (UPLC-MS/MS) was developed. The sample was extracted by ethyl acetate, cleaned up by florisil solid phase extraction (SPE), separated by C18 column and analyzed by UPLC-MS/MS under multiple reaction monitoring (MRM) mode via positive electrospray ionization, and the determination of aflatoxin was used external standard method. Results The deteciton limits of aflatoxin B1, B2, G1, and G2 0.04 μg/kg, and the limits of quantitation was 0.10 μg/kg. The method showed good linearity over the range of 0.1~20.0 μg/L with relative correlation coefficient of 0.9986, 0.9986, 0.9992, 0.9996. Conclusion The recoveries of aflatoxin B1, B2, G1, and G2 at spiked levels in the range of 0.1~5.0 μg/kg were79.1%~94.6% with relative standard deviations of 5.0 %~ 9.6%. The method showed practical, accurate and sensitive, and it is suitable for the determination of aflatoxin B1, B2, G1, and G2 in edible vegetable oil sample.
标题：超高压液相色谱-串联质谱法测定食用植物油中4种黄曲霉毒素B1、B2、G1、G2
英文标题：Determination of aflatoxin B1, B2, G1 and G2 in edible vegetable oil by ultra pressure liquid chromatography-tandem mass spectrometry
作者：
刘晓茂 秦皇岛出入境检验检疫局
李学民 秦皇岛出入境检验检疫局
王飞 秦皇岛出入境检验检疫局
张守军 秦皇岛出入境检验检疫局
杨志伟 秦皇岛出入境检验检疫局
曹彦忠 秦皇岛出入境检验检疫局
中文关键词:高压液相色谱-串联质谱,黄曲霉毒素,食用植物油,
英文关键词:ultra pressure liquid chromatography-tandem mass spectrometry (UPLC-MS/MS),aflatoxin,edible vegetable oil,
发表日期：2012-08-27
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