抗氧剂168的降解及其降解产物的测定  

Degradation of Irgafos 168 and Determination of Its Degradation Products

作　　者：杨岳平[1] 胡长鹰[1,2] 钟怀宁[3] 王志元[3] 曾广丰 

机构地区：[1]暨南大学食品科学与工程系,广东广州510632 [2]广东省普通高校产品包装与物流重点实验室,广东珠海519070 [3]广东出入境检验检疫局检验检疫技术中心,广东广州510623

出　　处：《现代食品科技》2016年第6期304-309,共6页Modern Food Science and Technology

基　　金：国家质检总局科技计划项目(2014IK078);国家自然科学基金(31571762;21277061)

摘　　要：抗氧剂168标准品及将其添加到聚丙烯薄膜中,经过紫外或微波处理均会发生降解,产生降解产物。以正己烷为提取溶剂,建立了聚丙烯薄膜中抗氧剂168及其降解产物2,4-二叔丁基苯酚和三(2,4-二-叔丁基苯基)磷酸酯的气相色谱-质谱检测方法。结果表明:三种物质分别在25~150 mg/L,0.02~20 mg/L,0.05~10 mg/L的浓度范围内线性关系良好,R^2分别为0.9990、0.9989、0.9955,回收率在81.83~115.21%之间,RSD在0.10~4.54%之间,检出限(LOD)分别为5.00μg/L,0.20μg/L和25.00μg/L,定量限(LOQ)分别为12.00μg/L,0.45μg/L和60.00μg/L,可见该方法精密度好,灵敏度高,定性定量准确,可用于聚丙烯中抗氧剂168及其两种降解产物的检测。将抗氧剂168添加到聚丙烯中经紫外、微波处理,降解率分别为31.88%、11.79%,产生3个降解产物,由标品确定其中两个为2,4-二叔丁基苯酚和三(2,4-二-叔丁基苯基)磷酸酯,推测另一个为抗氧剂168失去一个双叔丁基苯酚的产物;抗氧剂168标准品经紫外或微波处理,降解率均在5%以下。Tris（2,4-di-tert-butylphenyl）phosphite（Irgafos 168） alone and the Irgafos 168 added in the polypropylene（PP） films for food packing materials can generate degradation products under ultraviolet or microwave treatment. With n-hexane as the extraction solvent, a gas chromatography-mass spectrometry（GC-MS） method was developed for detecting Irgafos 168, and determining its degradation products, 2,4-di-tert-butylphenol and tris（2,4-di-tert-butylphenyl）phosphate, in PP food packing materials. The results showed that the calibration curves of three substances had a good linearity in the ranges of 25~150 mg/L, 0.02~20 mg/L, and 0.05~10 mg/L respectively, and the R2 values were 0.9990, 0.9989, and 0.9955, respectively. The spike recoveries at different spike concentration levels were in the range of 81.83~115.21% with RSD values in the range of 0.10~4.54%. The limits of detection（LOD） were 5.00 μg/L, 0.20 μg/L, and 25.00 μg/L, respectively, and the limits of quantitation（LOQ） were 12.00 μg/L, 0.45 μg/L, and 60.00 μg/L respectively. Therefore, this method is precise, highly sensitive, and accurate, and can be applied for detecting Irgafos 168, 2,4-di-tert-butylphenol, and tris（2,4-di-tert-butylphenyl）phosphate in PP. Irgafos 168 was added to PP, followed by ultraviolet and microwave treatments. The corresponding degradation rates were 31.88% and 11.7%, respectively, and three degradation products were generated. According to the standards, two of these degradation products were identified as 2,4-di-tert-butylphenol and tris（2,4-di-tert-butylphenyl）phosphate, and the other was speculated to be the result of Irgafos 168 with loss of the di-tert-butylphenol group. The degradation rate of Irgafos 168 standard was less than 5% under ultraviolet or microwave treatment.

关 键 词：聚丙烯(PP) 抗氧剂168 降解产物 气相色谱-质谱法(GC-MS) 

分 类 号：TS206.4[轻工技术与工程—食品科学] TQ325.14[轻工技术与工程—食品科学与工程]