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目的建立塑料饮用吸管中塑化剂迁移的气相色谱-质谱测定法。方法采用异辛烷在60℃条件下浸泡吸管试样1 h,将浸泡液浓缩后,用正己烷定容。采用气相色谱-质谱法(GC-MS)测定浓缩液中邻苯二甲酸二(2-乙基)己酯(DEHP)、邻苯二甲酸二正丁酯(DBP)和邻苯二甲酸二异壬酯(DINP),分别计算迁移量。结果在线性范围内,DEHP、DBP、DINP具有良好的线性关系,相关系数达0.999,加标回收率在87.3%~98.9%范围内,相对标准偏差为3.3%~7.6%;测定82批次吸管,DEHP和DBP迁移量检出率分别为52.4%和11.0%,DINP全部未检出。结论该方法线性关系良好,准确度和精密度满足实验要求,适用于塑料饮用吸管中塑化剂迁移的检测。
Objective To establish a gas chromatography-mass spectrometry method for plasticizer migration in plastic drinking straws. Methods The sample was soaked in isooctane at 60 ℃ for 1 h. After the soaking solution was concentrated, its volume was fixed with n-hexane. The concentration of di (2-ethylhexyl) phthalate (DEHP), di-n-butyl phthalate (DBP) and diisopropyl phthalate in the concentrated solution were determined by gas chromatography-mass spectrometry (GC- Nonyl ester (DINP) was used to calculate the migration volume. Results In the linear range, DEHP, DBP and DINP had a good linear relationship, the correlation coefficient was 0.999, the recoveries were within the range of 87.3% -98.9%, and the relative standard deviations were 3.3% -7.6% The detection rates of DEHP and DBP migration were 52.4% and 11.0%, respectively, and none of DINP was detected. Conclusion The method has a good linear relationship, the accuracy and precision meet the experimental requirements, and is suitable for the detection of plasticizer migration in plastic drinking straw.