LC-MS/MS法测定大米和食用油中的黄曲霉毒素

LC-MS /MS for determination of aflatoxin in rice and edible oil

目的利用高效液相色谱—质谱联用仪(LC-MS/MS)建立大米和食用油中黄曲霉毒素(B1、B2、G2、G1)的快速定性定量分析方法,为粮油食品中黄曲霉毒素的快速检测提供方法依据。方法选用Agilent ZORBAX Eclipse Plus C18色谱柱,以10 mmol/L甲酸铵-0.1%甲酸:甲醇为流动相,采用梯度洗脱进行分离。样品用甲醇水提取后,经过免疫亲和柱固相萃取,多重反应监测(MRM)方式检测。结果 AFG1和AFB1在1.0 ng/ml^21.0 ng/ml、AFG2和AFB2在0.3 ng/ml^6.5 ng/ml呈良好线性关系,平均回收率50%~92%。结论本方法无需衍生,灵敏度高,特异性强,可用于粮油食品中黄曲霉毒素的快速检测。

Objective To develop an ultra fast liquid chromatography—tandem mass spectrometry（LC-MS /MS） method for determination of aflatoxin（B 1,B 2,G 2,G 1） and provide proof for detection of aflatoxin in rice and edible oil.Methods Aflatoxin was extracted from rice and edible oil by methanol water,loaded on immnuoaffinity solid phase extraction column,and then separated on the Agilent ZORBAX Eclipse Plus C18 column with 10 mmol / L ammonium formate-0.1% formic acid and methanol as mobile phase by gradient elution.Detection was carried out by multiple reaction monitoring.Results AFG 1 and AFB 1 had a good linear result in the range of 1.0 ng / ml ~ 21.0 ng / ml,equally AFG 2 and AFB 2 in the range of 0.3 ng / ml ~ 6.5 ng / ml.The average recovery was 50% ~ 92%.Conclusion This method is sensitive,specific with no derived process.The assay is applied to a fast determination of aflatoxin in rice and edible oil.