Zhejiang Provincial Center for Disease Control and Prevention, Hangzhou, Zhejiang, China.
J Sep Sci. 2012 Nov;35(21):2932-9. doi: 10.1002/jssc.201200462. Epub 2012 Oct 12.
A quantified method for the determination of 17 phthalate esters (PAEs) in edible vegetable oil by GC-MS with the pretreatment of acetonitrile extraction and silica/N-(n-Propyl)ethylenediamine-mixed SPE column was established. By the quantification of internal standard of D(4)-di(2-ethylhexyl) phthalate, a good linearity range of related 17 PAEs was observed. The correlation coefficient was ranged at 0.9941.000, and the standard lowest quantified level was 0.050.15 mg/L. The spiking recoveries of 17 PAEs were 78.3108.9% with the relative standard deviations of 4.312.1% (n = 6). The method detection limits were 0.1~0.2 mg/kg. Meanwhile, PAEs were determined in 30 plastic buckets of edible vegetable oil from supermarkets in Hangzhou city of China. The survey of 30 oil samples showed di(2-ethylhexyl) phthalate (DEHP) had the 100% (30/30) detection rate. The levels of diisobutyl phthalate with 86.7% (26:30), di-n-butyl phthalate (DBP) with 70% (21:30) and diethyl phthalate with 10% (3:30) were detected. It was worth note that DBP with 16.7% (5:30) samples and DEHP with 10% (3:30) samples were beyond the regular migrating limit, which indicated that more attention should be paid to the PAEs in oil with plastic package.
建立了一种采用乙腈提取和硅胶/N-(正丙基)乙二胺混合 SPE 柱预处理，GC-MS 测定食用植物油中 17 种邻苯二甲酸酯（PAEs）的定量方法。通过 D（4）-二（2-乙基己基）邻苯二甲酸内标物的定量，观察到相关 17 种 PAEs 的良好线性范围。相关系数范围为 0.9941.000，标准最低定量水平为 0.050.15mg/L。17 种 PAEs 的加标回收率为 78.3108.9%，相对标准偏差为 4.312.1%（n=6）。方法检出限为 0.1~0.2mg/kg。同时，对杭州市超市 30 个塑料桶食用植物油中的邻苯二甲酸酯进行了测定。对 30 个油样的调查显示，二（2-乙基己基）邻苯二甲酸酯（DEHP）的检出率为 100%（30/30）。检测到二异丁基邻苯二甲酸酯的含量为 86.7%（26:30），二正丁基邻苯二甲酸酯（DBP）的含量为 70%（21:30），邻苯二甲酸二乙酯的含量为 10%（3:30）。值得注意的是，DBP 的 16.7%（5:30）和 DEHP 的 10%（3:30）样品超过了常规迁移限量，这表明应更加关注包装油中的邻苯二甲酸酯。
