摘要
采用高效液相色谱-串联质谱法同时测定间苯二甲胺、N-乙酰对氨基苯酚、4,4′-二氨基二苯砜、N,N′-二苯基硫脲在5种食品模拟物中的特定迁移量。水基模拟物样品过聚四氟乙烯(PTFE)过滤器后进样;油性(橄榄油)模拟物样品用20mmol·L^(-1)磷酸二氢钾溶液-甲醇(1+1)混合液振荡提取10min,提取液过PTFE过滤器后进样。采用C_(18)柱进行梯度洗脱分离,质谱分析中选择电喷雾离子源正离子及多反应监测模式。4种化合物的质量浓度在一定范围内与峰面积呈线性关系,测定下限(10S/N)在2.0~20μg·kg^(-1)之间。加标回收率在85.6%~108%之间,测定值的相对标准偏差(n=6)在0.90%~8.8%之间。用该方法检测实际样品,发现有N,N′-二苯基硫脲检出。
HPLC-MS/MS was applied to the determination of specific migrations of m-xylenediamine, acetyl- p-aminophenol, 4,4＇-diaminodiphenylsulfone arid thiocarbanilide in five types of food simulants. The aqueous food simulant samples were pretreated with polytetrafluoroethylene filter. The olive oil simulant samples were extracted by oscillation with a mixture of 20 mmol· L^-1 potassium dihydrogen phosphate solution and methanol （1＋1）, and the extract was treated with polytetrafluoroethylene filter. Then the mixture of m-xylenediamine, acetyl-paminophenol, 4,4r-diaminodiphenylsulfone and thiocarbanilide was separated on a C18 column by gradient elution, ESI＋ and MRM were adopted in MS analysis. Linear relationships were found between the peak areas and the mass concentrations of the four compounds in defined ranges, with the lower limits of determination in the range of 2.0- 20 μg· kg^-1. Recovery rates obtained by standard addition method were in the range of 85.6%-108%, and RSDs （n=6） were in the range of 0. 90%-8. 8%. Thiocarbanilide was found out in the real samples by this mehod.
出处
《理化检验（化学分册）》
CAS
CSCD
北大核心
2017年第3期263-269,共7页
Physical Testing and Chemical Analysis(Part B:Chemical Analysis)
