固相萃取-气相色谱质谱联用法同时测定食品接触产品中邻苯基苯酚、噻苯咪唑、联苯及抑霉唑的迁移量

摘要

A novel SPE-GC-MS method of determination of ortho-phenylphenol,thiabendazole,biphenyl and imazalil in food stimulants was developed. Samples were immersed in stimulants(H2O,4% acetic acid,20% ethanol and 50% etha⁃nol),and kept in incubator at 60℃ in a duration of 2h. The immersed solutions were purified by SPE micro column before the penetration through a 0.45-μm microporous membrane. And then the purified solutions were injected into GC-MS polar column. With external standard method,the values were gotten by MS detection. Under the optimum conditions,the cali⁃bration curves were linear from 2 to 800 μg/L with LOQs(S/N = 10)of 3,5,2 and 5 μg/L for OPP,TBZ,DB,IMZ,re⁃spectively. The method provided recoveries of 70.4 % -112 % in three kinds of spiked concentrations,and the RSD of were between 1.78 % and 6.72 %. The satisfied experimental results indicated that the proposed method can be directly used for determination of OPP,TBZ,DB and IMZ in food stimulants conveniently,rapidly,reproducibly and accurately.%建立了气相色谱质谱联用技术同时测定邻苯基苯酚（OPP）、噻苯咪唑（TBZ）、联苯（DP）及抑霉唑（IMZ）迁移量的方法。样品分别采用水、4%乙酸、20%乙醇、50%乙醇作为食品模拟物，在特定条件下浸泡提取。浸泡液运用固相萃取技术净化提纯后过0.45μm 微孔薄膜，在微极性柱上进行分离，质谱检测，外标法定量分析。优化条件下， OPP、TBZ、DP、IMZ在2-800μg/L浓度范围内与其峰面积线性良好，定量限分别为3、5、2和5μg/L（S/N=10）。在3个浓度水平进行添加实验，OPP、TBZ、DP、IMZ的平均回收率在70.4-112%之间，重复性精密度在1.78-6.72%（n=6）之间。结果表明，本方法操作简单快速、重现性好、准确度高。