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  

Determination of Ortho-phenylphenol,Thiabendazole,Biphenyl and Imazalil in food stimulants by SPE-GC-MS

作　　者：陈旻实[1] 林星辉[2] 郑洁[1] 郑思远[1] 陈佳敏[1] 张灵玲[2] 

机构地区：[1]福建出入境检验检疫局技术中心,国家消费品安全检测重点实验室,福建省检验检疫技术研究重点实验室,福建福州350003 [2]福建农林大学生命科学学院,福建福州350002

出　　处：《福建分析测试》2015年第1期1-5,共5页Fujian Analysis & Testing

基　　金：福建出入境检验检疫局科技计划项目(FK2012-30)

摘　　要：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。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% ethanol）, 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 calibration 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, respectively. 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.

关 键 词：邻苯基苯酚 噻苯咪唑 联苯 抑霉唑 食品接触产品 气相色谱质谱联用 迁移 

分 类 号：O657.71[理学—分析化学]