固相萃取-高效液相色谱法测定塑料桶装食用油中的酞酸酯类增塑剂

Determination of Phthalate Acid Esters in Plastic Bottled Edible Oil by Solid-phase Extraction Coupled with HPLC

为检测塑料桶装食用油中酞酸酯类(PEAs)增塑剂的污染现状,以自制弗罗里硅土固相萃取柱对食用油样品中PEAs进行富集净化处理后,选用Waters syrrvnetry C_(18)柱(4.6 mm×250 mm,5μm)反相分离,甲醇-水作流动相梯度洗脱,紫外波长227 nm检测。结果表明:邻苯二甲酸二乙酯通过对无锡市场上销售的几种品牌的塑料桶装食用油样品的测定,发现其中邻苯二甲酸二丁酯(DBP)和邻苯二甲酸二辛酯(DOP)的最高含量分别为6.72 mg/ kg和24.16 mg/kg,测定的结果通过液相色谱-质谱分析确证。方法回收率:邻苯二甲酸二乙酯(DEP)为88.46%～95.37%,DBP为77.39%～102.63%,DOP为80.11%～94.19%,DEP、DBP和DOP的定量测定的相对标准偏差分别为2.53%、2.56%和4.99%。因此,食用油包装材料中的增塑剂会溶移到食用油中。

To investigate phthalate acid esters（PAEs） of edible oil in plastic container. Methods ： A florisil solid phase extraction column was prepared to enrich and purify PAEs followed by reverse phase Waters symmetry C18（4.6×250mm,5μm）HPLC. Methanol-water was used as mobile phase eluent under gradient conditions and detection was carried out with an UV detector at 230nm. Several kinds of edible oil in plastic container on the Wuxi market were used as samples. The maximum level of DBP and DOP in edible oil were 6.72mg/kg and 24.16mg/kg respectively. This results were confirmed by HPLC-MS. The recoveries were DEP 88.46%-95.37% ,DBP 77.39%-102.63%,DOP 0.11%-94.19% ,the RSDS were 2.53%,2.58%, 4.99% respectively. Conclusion： Plasticizer in the container could be dissolved and transferred into edible oil. Therefore, it＇s necessary to conduct safety evaluation and establish its threshold in edible oil. The proposed method was simple and rapid; the results were accurate and reproducible.