摘要
提出了同位素稀释高效液相色谱-串联质谱法测定植物性食品中的杂色曲霉素。植物性食品样品经乙腈-水混合液提取,提取液通过HLB SPE小柱净化并浓缩后,样品溶液在反相液相色谱柱上分离。MS/MS分析中采用电喷雾离子源离子化和多反应离子监测(MRM)检测,并用同位素稀释内标法定量。杂色曲霉素的线性范围在0.5~100μg·L^(-1)之间,其线性相关系数大于0.999。小麦和玉米样品的测定下限(10S/N)为0.5μg·kg^(-1),花生和黄豆样品的测定下限(10S/N)为0.8μg·kg^(-1)。以不同的植物性食品作为基体,分别加入不同浓度水平的杂色曲霉素标准液,按方法进行回收试验,测得回收率在88.2%~105%之间;测定值的日内相对标准偏差(n=6)小于7.5%,日间相对标准偏差(n=3)小于9.0%。
A method was proposed for the determination of sterigmatocystin in plant food with isotope diution internal standard hy HPLC-MS/MS. Sample of plant food was extracted with a mixture of acetonitrile and water. The extract was purified on HLB SPE microcolumn. The purified extract was concentrated and then separated on RP-LC column. ESI and MRM were adopted in MS/MS analysis and isotope dilution internal standard was used for quantification. Linearity range for sterigmatocystin was found between 0. 5- 100 μg·L^-1 with correlation coefficient greater than 0. 999. Values of lower limits of determination （10S/N） found for wheat and maize were same to be 0. 5μg·kg^-1 , and for peanut and soybean were same to be 0. 8μg·kg^-1. Standard sterigmatocystin of different concentration levels was added to various matrixes of plant food, and tests for recovery were made, giving values of recovery in the range of 88.2%- 105%. Values of intra-day RSDs （n=6） found were less than 7.5% and of inter-day RSDs （n=3） found were less than 9.0%.
出处
《理化检验（化学分册）》
CAS
CSCD
北大核心
2016年第9期1112-1116,共5页
Physical Testing and Chemical Analysis(Part B:Chemical Analysis)
