Department of Analytical Chemistry, Almeria University, Almeria, Spain.
J Sep Sci. 2010 Mar;33(4-5):502-8. doi: 10.1002/jssc.200900663.
A rapid and simple method was developed to determine aflatoxins B1, B2, G1, G2 and ochratoxin A in animal feed and pet foods by UHPLC-MS/MS. Because the complexity of the evaluated matrices, the proposed method is based on sonication extraction using an ACN/water mixture (80:20 v/v) followed by a clean-up step utilising C(18) as sorbent. Performance parameters of the method were evaluated, including linearity, trueness, precision and LOQ. Good linearity was found for all mycotoxins, with determination coefficients higher than 0.99 in the range considered, using matrix-matched calibration for quantification purposes. Recoveries ranged from 84 to 113%, with RSD lower than 20%, whereas LOQs were 5 microg/kg for the assayed mycotoxins. Finally, the method was successfully applied to the analysis of 19 real samples, detecting aflatoxin G2 in two samples at 13 and 17 microg/kg respectively, whereas the other mycotoxins were detected at trace levels (<LOQ) in five samples.
建立了一种超高效液相色谱-串联质谱法(UHPLC-MS/MS),用于快速、简单地检测动物饲料和宠物食品中的黄曲霉毒素 B1、B2、G1、G2 和赭曲霉毒素 A。由于评价基质的复杂性,该方法基于使用 ACN/水混合物(80:20 v/v)进行超声提取,然后使用 C(18)作为吸附剂进行净化步骤。对该方法的性能参数进行了评估,包括线性、准确性、精密度和定量限。对于所有真菌毒素,均发现具有良好的线性,在考虑的范围内,使用基质匹配校准进行定量,其决定系数均高于 0.99。回收率在 84%至 113%之间,RSD 低于 20%,而测定的真菌毒素的定量限为 5μg/kg。最后,该方法成功地应用于 19 个实际样品的分析,在两个样品中分别检测到黄曲霉毒素 G2 的含量为 13μg/kg 和 17μg/kg,而在五个样品中,其他真菌毒素的含量则低于检测限(<LOQ)。