液相色谱-串联质谱法分析花生油中的黄曲霉毒素  

Determination of Aflatoxin in Peanut Oil by Liquid Chromatography-Tandem Mass Spectrometry

作　　者：黄小小 莫秋云 HUANG Xiaoxiao;MO Qiuyun(Hezhou City Center for Disease Control and Prevention,Hezhou 542800,China;Hezhou Inspection and Testing Center,Hezhou 542899,China)

机构地区：[1]贺州市疾病预防控制中心,广西贺州542800 [2]贺州市检验检测中心,广西贺州542899

出　　处：《食品安全导刊》2024年第6期113-115,131,共4页China Food Safety Magazine

摘　　要：目的:建立一种样品前处理简易、快速、成本低的液相色谱-串联质谱法,对花生油样品中黄曲霉毒素进行定量分析。方法:花生油样品经甲醇-水(7∶3)提取,以10 mmol·L^(-1)乙酸铵溶液-甲醇作为流动相进行梯度淋洗,采用电喷雾正离子模式多反应监测扫描,外标法定量。利用所建立的分析方法对样品进行高、中、低3水平的加标实验,并对实际样品中黄曲霉毒素含量进行测定。结果:黄曲霉毒素B1、B2、G1、G2在0.2~10.0 ng·mL^(-1)呈现良好的线性相关性,相关系数分别为0.999 6、0999 5、0.998 8、0.999 7;加标回收率在72.5%~102.4%;检出限分别为0.02μg·kg^(-1)、0.02μg·kg^(-1)、0.01μg·kg^(-1)、0.03μg·kg^(-1);相对标准偏差均<9.2%,符合国标要求。利用该方法对实际样品中黄曲霉毒素含量进行测定,所得结果与GB 5009.22—2016中的第一法同位素稀释液相色谱-串联质谱法相近。结论:该方法在确保准确度的前提下,具有较好的选择性和高灵敏度,准确高效,可用于花生油中黄曲霉毒素的检测。Objective:To establish a simple,rapid and low-cost liquid chromatography-tandem mass spectrometry method for quantitative analysis of aflatoxins in peanut oil samples.Method:Peanut oil samples were extracted by methanol-water(7∶3),and gradient elution was carried out with 10 mmol·L^(-1) ammonium acetate solution-methanol as mobile phase.Electrospray positive ion mode multiple reaction monitoring scanning was used,and external standard method was used for quantitative analysis.The established analytical method was used to carry out high,medium and low three levels of standard addition experiments on samples,and the content of aflatoxin in actual samples was determined.Result:Aflatoxin B1,B2,G1,G2 showed good linear correlation in the range of 0.2~10.0 ng·mL^(-1),the correlation coefficients were 0.9996,0.9995,0.9988,0.9997 respectively.The recovery was 72.5%~102.4%.The detection limits were 0.02μg·kg^(-1),0.02μg·kg^(-1),0.01μg·kg^(-1),0.03μg·kg^(-1),respectively.The relative standard deviation was less than 9.2%,which met the requirements of national standard.The method was used to determine the content of aflatoxin in actual samples,and the results were similar to those of the first method of GB 5009.22—2016 isotope dilution liquid chromatography-tandem mass spectrometry.Conclusion:This method has good selectivity,high sensitivity,accuracy and high efficiency under the premise of ensuring accuracy,and can be used for the detection of aflatoxin in peanut oil.

关 键 词：花生油 黄曲霉毒素 液相色谱-串联质谱法 

分 类 号：O657.63[理学—分析化学] TS225.12[理学—化学]