超高效液相色谱串联飞行时间质谱法检测黑水虻产品中黄曲霉毒素B1

本研究建立了黑水虻产品中黄曲霉毒素B1(AFB1)的超高效液相色谱串联四级杆飞行时间质谱测定方法,对黑水虻幼虫粉中AFB1的提取、超高效液相色谱串联质谱检测条件进行了优化。使用甲醇-水溶液(8:2,体积比),添加7%氯化钠对黑水虻幼虫粉中AFB1进行提取,免疫亲和柱净化,甲醇-乙酸铵(10 mmol/L)水溶液作为流动相进行梯度洗脱,电喷雾离子源(ESI)正离子模式检测,7.0 min出峰。结果表明:AFB1在1~20μg/kg浓度范围内线性关系良好,相关系数大于0.999,幼虫粉回收率为83.1%~118.3%,相对标准偏差(RSD)为6%~10%;虫粪回收率为76.6%~114.1%,相对标准偏差(RSD)为0~3%;检出限(LOD,S/N≥3)为0.01μg/kg,定量限(LOQ,S/N≥10)为0.05μg/kg。该方法操作简单、结果准确,可以用于黑水虻幼虫粉和虫粪产品中AFB1的检测。

Determination of aflatoxin B1 in black soldier fly products by UPLC-Q-TOF/MS

To establish the UPLC-Q-TOF/MS methods for determination of aflatoxin B1(AFB1) in black soldier fly products including larvae powder and larvae feces, parameters on AFB1 extraction, purification and determination were optimized in this study. The AFB1 was extracted with 80% methanol containing 7% NaCl, purification of aflatoxin immune affinity. The mobile phase by gradient elution was 10 mmol/L ammonium acetate and methanol.ESI positive ion mode was used and the retention time of AFB1 was 7.0 min. The results showed that a high correlation coefficient(r2>0.999) of AFB1 was obtained within linear range(1~20 μg/kg). Black soldier fly larvae powder recoveries were ranged from 83.1%~118.3%. The relative standard deviation(RSD) was within 6%~10%. Larvae feces recoveries were ranged from 76.6%~114.1%. The relative standard deviation(RSD) was within 0~3%. The detection limit(LOD, S/N≥3) was 0.01 μg/kg. The quantification limit(LOQ, S/N≥10) was 0.05 μg/kg. These methods were simple, accurate and suitable for the rapid detection of AFB1 in black soldier fly larvae powder and larvae feces.