摘要
目的 建立基于挥发性铵盐盐析辅助液液萃取结合超高效液相色谱-串联质谱法检测酱油中黄曲霉毒素B、B、G、G4种黄曲霉毒素含量的分析方法。方法 酱油样品用乙腈提取,乙酸铵作为盐析助剂分层,提取液加水定容后,采用C反相色谱柱以5 mmol/L乙酸铵溶液-甲醇/乙腈为流动相进行梯度洗脱,采用电喷雾正离子模式检测,外标法定量。实验考察了萃取溶剂、盐析助剂及pH对萃取效率的影响。结果 最优实验条件下,在0.5~20.0 ng/mL范围内4种黄曲霉毒素线性良好,相关系数均大于等于0.999,检出限为0.01~0.04μg/kg,定量限为0.03~0.12μg/kg;对空白酱油样品进行0.8、4.0、8.0μg/kg3个水平的加标实验,回收率为73.2%~94.5%,相对标准偏差为0.9%~5.9%。结论 该方法操作简捷、成本低、准确度高,可满足对酱油中4种黄曲霉毒素的快速准确分析要求。
Objective To establish an analytical method for the determination of aflatoxins B, B, Gand Gin soy sauce based on volatile ammonium salt salting-out assisted liquid-liquid extraction combined with ultra performance liquid chromatography-tandem mass spectrometry. Methods The soy sauce sample was extracted with acetonitrile, and ammonium acetate was used as the salting-out aid for stratification, after the extraction solution was fixed in volume by adding water, gradient elution was performed using a Creverse-phase chromatographic column with 5 mmol/L ammonium acetate solution–methanol/acetonitrile as the mobile phase, and electrospray positive ion mode detection was adopted, followed by external standard quantification. The effects of extraction solvent,salting-out aid and pH on extraction efficiency were investigated. Results Under the optimal experimental conditions, the linearity of the 4 kinds of aflatoxins were good in the range of 0.5-20.0 ng/mL, the correlation coefficients were all greater than or equal to 0.999, and the limits of detection were 0.01-0.04 μg/kg, and the limits of quantitation were 0.03-0.12 μg/kg;the standard addition experiments at the 3 levels of 0.8, 4.0 and 8.0 μg/kg were performed on the blank soy sauce sample, and the recovery rates were 73.2%-94.5%, and the relative standard deviations were 0.9%-5.9%. Conclusion This method is simple, low in cost and high in accuracy, and can meet the requirements of rapid and accurate analysis of 4 kinds of aflatoxins in soy sauce.
作者
王东旭
王新财
王凤丽
胡奇杰
厉芬
WANG Dong-Xu;WANG Xin-Cai;WANG Feng-Li;HU Qi-Jie;LI Fen(Huzhou Institute for Food and Drug Control,Huzhou 313000,China)
出处
《食品安全质量检测学报》
CAS
北大核心
2022年第14期4634-4640,共7页
Journal of Food Safety and Quality
基金
浙江省市场监督管理局科研计划项目(20200124、20190338)
湖州市科技计划项目(2019GZ30、2021GZ29)。
关键词
酱油
黄曲霉毒素
盐析辅助液液萃取
soy sauce
aflatoxin
salting-out assisted liquid-liquid extraction
