高效液相色谱法同时检测粮谷中的黄曲霉毒素和赭曲霉毒素

建立粮谷类食品中黄曲霉毒素(B1、B2、G1 和G2)和赭曲霉毒素A 的同时检测方法。样品经过甲醇- 水(80:20，V/V)提取，液液萃取净化和富集后，三氟乙酸衍生，采用Agilent ZORBAX SB-C18 色谱柱(4.6mm ×250mm)，以乙腈和体积分数2% 冰醋酸溶液为流动相梯度洗脱，在线变换波长荧光检测。根据3 倍信噪比的峰响应值，确定黄曲霉毒素(B1、B2、G1 和G2)和赭曲霉毒素A 检出限分别为0.06、0.03、0.18、0.05μg/kg 和0.51μg/kg，上述5 种毒素分别在质量浓度0.05～100、0.125～25.00、0.05～100、0.125～25.00μg/L 和0.05～50.00μg/L 范围内呈线性相关，相关系数r 分别为0.9998、0.9998、0.9998、0.9996 和0.9998；在玉米、大米、小麦3 类样品中加标回收率平均为71.73%～115.37%，相对标准偏差为3.00%～9.88%，方法学验证结果表明，黄曲霉毒素和赭曲霉毒素A 5 种毒素同时检测结果与现行国标的单独检测方法检测结果无显著性差异(P ＞ 0.05)。

Simultaneous Determination of Aflatoxins and Ochratoxin A in Cereal Grains by High Performance Liquid Chromatography

A HPLC method was developed for the simultaneous determination of aflatoxins B1, B2, G1 and G2 and ochratoxin A in cereal grains. Cereal grain samples were subject to extraction using methano1-water (80:20, V/V), liquid-liquid purification, enrichment and derivation using trifluoroacetic acid. The purification was performed on an Agilent ZORBAX SB-C18 column (4.6 mm × 250 mm) with a linear gradient elution of acetonitrile-2% glacial acetic acid. The detection limits of developed HPLC method for AFB1, AFB2, AFG1, AFG2 and OTA were 0.06, 0.03, 0.18, 0.05μg/kg and 0.51μg/kg, respectively. The linear detection ranges of developed HPLC method for AFB1, AFB2, AFG1, AFG2 and OTA was 0.05－100, 0.125－25.00, 0.05－100, 0.125 － 25.00μg/L and 0.05 － 50.00μg/L with correlation coefficients of 0.9998, 0.9998, 0.9998, 0.9996 and 0.9998, respectively. Recovery rates in cereal grains (corn, rice, wheat) spiked with mycotoxins were in the range of 71.73%－115.37% with the relative standard deviation of 3.00% － 9.88%. This HPLC method exhibited the capability to simultaneously determinate mycotoxins. Moreover, no significant difference was observed between the determination results and current national standard (P＞ 0.05).