UPLC-MS/MS测定普洱茶中黄曲霉毒素B1,B2,G1和G2

Determination of Aflatoxin B1, B2, G1 and G2 in Pu’er Tea by UPLC-MS/MS

为建立超高效液相色谱-串联三重四级杆质谱法测定普洱茶中黄曲霉毒素B1, B2, G1和G2的方法,普洱茶中的黄曲霉毒素经70%甲醇水溶液超声提取,免疫亲和柱萃取柱净化,以电喷雾正离子串联质谱多反应监测模式(MRM)进行检测,外标法定量。结果表明,黄曲霉毒素B1和G1在0.1~8 ng/mL浓度范围内呈良好线性关系,相关系数在0.999 4~0.999 6之间,黄曲霉毒素B2和G2在0.15~2.4 ng/mL浓度范围内呈良好线性,相关系数在0.999 0~0.999 1之间;在高、中、低3个浓度进行加标, AFTB1和AFTG1加标量为1.25, 25和100 ng, AFTB2和AFTG2加标量为3.75, 7.5和30 ng,回收率为80.3%~116.7%,相对标准偏差≤5.2%(n=6);黄曲霉毒素B1, B2, G1和G2的检出限均为0.25μg/kg,定量限分别为0.60, 0.60, 0.60和0.80μg/kg。该方法专属性强、操作简单、灵敏度高、准确,适用于普洱茶中黄曲霉毒素B1, B2,G1和G2的检测。

A method for the determination of aflatoxin B1, B2, G1 and G2 in Pu’er tea was established by super high performance liquid chromatography series three weight four grade mass spectrometry. Aflatoxin in Pu’er tea was extracted by ultrasonic extraction of 70% methanol solution, purified by immunoaffinity column, and detected by electrospray ionization tandem mass spectrometry(MRM). The external standard method was used for quantitative analysis. The results show that aflatoxin B1 and G1 in the 0.1-8 ng/mL range show a good linear relationship, whose correlation coefficients are 0.999 6-0.999 4, and aflatoxin B2 and G2 in the 0.15-2.4 ng/mL range show a good linear correlation coefficient, whose ranges are 0.999 0-0.999 1;For the three concentrations of high, medium and low, AFTB1 and AFTG1 are added as 1.25, 25 and 100 ng, and AFTB2 and AFTG2 are added as 3.75, 7.5 and 30 ng. The recovery rate is 80.3%-116.7%, and the relative standard deviation is less than 5.2%(n=6);The limits of detection of aflatoxin B1, B2, G1 and G2 are 0.25 g/kg, and the limits of quantitation are 0.60, 0.60, 0.60 and 0.80 g/kg. This method is suitable for the detection of aflatoxin B1, B2, G1 and G2 in Pu’er tea, with high specificity, simple operation, high sensitivity and accuracy.