Wu Ping-gu, Yang Da-jin, Shen Xiang-hong, Pan Xiao-dong, Wang Li-yuan, Zhang Jing, Tan Ying, Feng Liang, Ying Ying
Institute of Physical and Chemical Inspection, Zhejiang Provincial Center for Disease Control and Prevention, Hangzhou 310051, China.
Zhonghua Yu Fang Yi Xue Za Zhi. 2012 Jun;46(6):561-6.
We aimed to establish a quantified method for the 17 phthalate acid esters (PAE) in edible vegetable oil by gas chromatography-mass spectrometry (GC-MS) with the pretreatment of acetonitrile extraction and silica/N-(n-propyl)ethylenediamine (silica/PSA) mixed solid phase extraction column and evaluated the PAE of 25 edible oil samples from supermarkets in Hangzhou city.
The internal standard solution (D4-DEHP) was added in edible vegetable oil sample. The analytes were extracted by acetonitrile with 1 min vortex, and centrifuged at 3050×g for 5 min. The supernatant was then cleaned with silica/PSA column, and eluted with acetonitrile. The elution was dried with N2 flow at 50°C and diluted to 1.0 ml with hexane. Then, 17 PAE were tested by GC-MS and quantified with internal standards. The repeatability and sensitivity of the assay were evaluated. PAE were then determined in 25 plastic buckets of edible vegetable oil from supermarkets in Hangzhou city.
By the quantification of internal standard of D4-DEHP, a good linearity range of related 17 PAE was observed. The correlation coefficient was 0.994-1.000 and the standard lowest quantified level was 0.05-0.15 µg/ml. The spiking recoveries of 17 PAE were 78.3%-108.9% with the RSD of 4.3%-12.1% (n=6). The method detection limits were 0.1-0.2 mg/kg. In 25 plastic buckets of edible vegetable oil from Hangzhou, DMP, DEP, DIBP, DBP and DEHP were detected at the range of <0.1-1.8 mg/kg and the detection rates were 12% (3/25), 24% (6/25), 100% (25/25), 96% (24/25) and 100% (25/25), respectively. Other 12 PAE was not detected. For DBP with the level of <0.1 to 1.3 mg/kg, the results of 16% (4/25) samples exceeded the regular migrating limit of 0.3 mg/kg. For DEHP of <0.2-1.8 mg/kg, the data of 12% (3/25) samples were beyond the regular migrating limit of 1.5 mg/kg.
The pretreatment by silica/PSA mixed solid phase extraction column can satisfy the PAE determination requirements in edible vegetable oils. The DMP, DIBP, DEP, DBP and DEHP were detected from the survey of 25 edible oil samples in Hangzhou city.
旨在建立一种采用气相色谱 - 质谱联用仪（GC - MS），经乙腈萃取及硅胶/N -（正丙基）乙二胺（硅胶/PSA）混合固相萃取柱预处理后，测定食用植物油中17种邻苯二甲酸酯（PAE）的定量方法，并对杭州市超市采集的25份食用油样品中的PAE进行评估。
向食用植物油样品中加入内标溶液（D4 - DEHP）。用乙腈对分析物进行1分钟涡旋萃取，然后在3050×g条件下离心5分钟。上清液再用硅胶/PSA柱净化，并用乙腈洗脱。洗脱液在50°C下用氮气吹干，并用正己烷稀释至1.0 ml。然后，通过GC - MS检测17种PAE并用内标进行定量。评估该测定方法的重复性和灵敏度。随后测定杭州市超市25个塑料桶装食用植物油中的PAE。
通过D4 - DEHP内标定量，观察到17种相关PAE具有良好的线性范围。相关系数为0.994 - 1.000，最低定量标准水平为0.05 - 0.15μg/ml。17种PAE的加标回收率为78.3% - 108.9%，相对标准偏差（RSD）为4.3% - 12.1%（n = 6）。方法检测限为0.1 - 0.2 mg/kg。在杭州市25个塑料桶装食用植物油中，检测到邻苯二甲酸二甲酯（DMP）、邻苯二甲酸二乙酯（DEP）、邻苯二甲酸二异丁酯（DIBP）、邻苯二甲酸二丁酯（DBP）和邻苯二甲酸二（2 - 乙基己基）酯（DEHP），含量范围为<0.1 - 1.8 mg/kg，检出率分别为12%（3/25）、24%（6/25）、100%（25/25）、96%（24/25）和100%（25/25）。其他12种PAE未检出。对于含量<0.1至1.3 mg/kg的DBP，16%（4/25）的样品结果超过了0.3 mg/kg的常规迁移限量。对于含量<0.2 - 1.8 mg/kg的DEHP，12%（3/25）的样品数据超出了1.5 mg/kg的常规迁移限量。
硅胶/PSA混合固相萃取柱预处理能满足食用植物油中PAE的测定要求。在对杭州市25份食用油样品的检测中，检测到了DMP、DIBP、DEP、DBP和DEHP。
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