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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。
Antioxidant 168 standard and added to the polypropylene film, after UV or microwave treatment will occur degradation, resulting in degradation products. Gas chromatography of antioxidant 168 and its degradation products 2,4-di-tert-butylphenol and tris (2,4-di-t-butylphenyl) phosphate was established with n-hexane as the extraction solvent Mass spectrometry method. The results showed that there was a good linear relationship between the three substances in the concentration range of 25 ~ 150 mg / L, 0.02 ~ 20 mg / L and 0.05 ~ 10 mg / L respectively, with the R ~ 2 values of 0.9990, 0.9989 and 0.9955, The detection limits (LODs) were 5.00μg / L, 0.20μg / L and 25.00μg / L respectively. The limits of quantification (LOQ) were between 12.83 and 115.21% , 0.45μg / L and 60.00μg / L, respectively. It can be seen that this method has good precision, high sensitivity and accurate qualitative and quantitative determination. It can be used for the detection of antioxidants 168 and two degradation products in polypropylene. The antioxidant 168 was added to the polypropylene by UV, microwave treatment, the degradation rates were 31.88%, 11.79%, resulting in three degradation products identified by the standard two of them 2,4-di-tert-butyl phenol and Tris (2,4-di-t-butylphenyl) phosphate, presumably the other one is a product of bis-t-butylphenol lost by antioxidant 168; the antioxidant 168 standard treated by UV or microwave, the degradation rate Below 5%.