食用花生油中16种邻苯二甲酸酯类塑化剂的GPC-GC-MS检测方法研究

Study on the GPC-GC-MS Detection Method of 16 Kinds of Phthalic Acid Ester Plasticizers in Edible Peanut Oil

[目的]建立一种适用于花生油中邻苯二甲酸酯类化合物的测定方法,为塑化剂的安全评估提供依据。[方法]利用凝胶渗透色谱(GPC)对花生油样品进行净化,采用气相色谱-质谱(GC-MS)联用技术结合选择离子扫描模式(SIM)对样品中16种邻苯二甲酸酯类化合物进行定性和定量分析。[结果]邻苯二甲酸酯标准溶液在0.5~8.0 mg/L质量浓度范围内呈良好线性关系,相关系数(r)不低于0.999,检出限(S=3N)为0.02~0.05 mg/kg。添加水平为0.5、1.0、2.0 mg/kg时,平均回收率为78.3%~97.6%,相对标准偏差(RSD,n=3)为2.4%~7.2%。[结论]该方法操作简单、灵敏、准确,可用于食用花生油中邻苯二甲酸酯类化合物的检测。

[Objective]To establish a method for the determination of phthalic acid esters in peanut oil.[Method]Gel permeation chromatography(GPC)was used to purify peanut oil samples.Qualitative analysis and quantitative analysis of 16 kinds of phthalic acid esters(PAEs)compounds in samples were carried out by gas chromatography-mass spectrometry(GC-MS)combined with selective ion scanning mode(SIM).[Result]The results showed that the standard solution of phthalic acid esters(PAEs)showed a good linearity in the range of 0.5-8.0 mg/L mass concentration,and the correlation coefficient(R)was not less than 0.999,and the detection limit(S=3N)was 0.02-0.05 mg/kg.When adding levels were 0.5,1.0 and 2.0 mg/kg,the average recovery rate was 78.3%-97.6%,and the relative standard deviation(RSD,n=3)was 2.4%-7.2%.[Conclusion]The method is simple,sensitive and accurate,and can be used for the detection of phthalic acid esters in edible peanut oil.