摘要
粉碎的婴幼儿辅助饼干食品样品经体积比为89∶10∶1的乙腈-水-乙酸混合液提取,采用净化剂为50mg十八烷基硅烷、30mg N-丙基乙二胺和30mg氨丙基的QuEChERS方法净化,采用高效液相色谱-串联质谱法测定净化液中黄曲霉毒素B1、黄曲霉毒素B2、黄曲霉毒素G1、黄曲霉毒素G2、O-甲基柄曲霉素、柄曲霉素、黄曲霉毒素M1、黄曲霉毒素M2等8种黄曲霉毒素及其同系物的含量。以AQ-C18HP色谱柱(2.1mm×100mm,3.0μm)为固定相,以不同体积比的含5mmol·L^-1乙酸铵的0.1%(体积分数)甲酸溶液和甲醇的混合液为流动相进行梯度洗脱,串联质谱分析中采用电喷雾离子源正离子扫描模式和多反应监测模式。8种黄曲霉毒素及其同系物的质量浓度在一定范围内与其对应的峰面积呈线性关系,检出限(3S/N)为0.05~0.10μg·kg^-1,测定下限(10S/N)为0.15~0.30μg·kg^-1。以空白样品为基体进行加标回收试验,所得回收率为76.3%~95.9%,测定值的相对标准偏差(n=6)为3.1%~11%。
The crushed sample of supplementary cookies for infants and young children was extracted with mixture of acetonitrile,water and acetic acid with volume ratio of 89∶10∶1,and purified by QuEChERS method with purification agents of 50 mg ODS,30 mg PSA and 30 mg NH2.HPLC-MS/MS was applied to the determination of 8 aflatoxins and their homologues,i.e.AFB1,AFB2,AFG1,AFG2,MST,ST,AFM1 and AFM2 in the purified liquid.AQ-C18 HP chromatographic column(2.1 mm×100 mm,3.0μm)was used as stationary phase,and the mixture of 0.1%(φ)formic acid solution containing 5 mmol·L^-1 ammonium acetate and methanol mixed in different ratios was used as mobile phase in gradient elution.ESI+and multi-reactions monitor mode were adopted in MS/MS.Linear relationships between values of peak area and mass concentration of the 8 aflatoxins and their homologues were kept in definite ranges,with detection limits(3 S/N)in the range of 0.05-0.10μg·kg^-1 and lower limits of determination(10 S/N)in the range of 0.15-0.30μg·kg^-1.On the base of blank sample,test for recovery was made by standard addition method;values of recovery found were in the range of 76.3%-95.9%,with RSDs(n=6)of determined values in the range of 3.1%-11%.
作者
张艾青
ZHANG Aiqing(Shandong Vocational Animal Science and Vetevinary College,Weifang 261061,China)
出处
《理化检验（化学分册）》
CAS
CSCD
北大核心
2020年第5期570-576,共7页
Physical Testing and Chemical Analysis(Part B:Chemical Analysis)
基金
潍坊市科学技术发展计划项目(2018GX056)。
作者简介
张艾青,讲师,研究方向为食品科学,E-mail:zhangaiqingwf@163.com。
