不同类别食品中21种邻苯二甲酸酯的气相色谱-质谱测定及其分布情况研究

Study on Determination of 21 Phthalate Acid Esters and Their Distributions in Different Types of Foods by Gas Chromatography-Mass Spectrometry

首次建立了同时测定不同类别食品中21种邻苯二甲酸酯的气相色谱-质谱(GC-MS)分析方法。对各种类别的食品采取不同的分离、净化方法;优化了成分复杂的香精或植物提取物等样品的色谱测定条件,通过提取特征离子进行检测和确证,消除了基质干扰,避免产生假阳性结果;探讨了邻苯二甲酸酯类的质谱碎裂机理。21种邻苯二甲酸酯的质量浓度在0.1～100 mg/L范围内呈良好线性,相关系数(r)不低于0.999 2,方法的定量下限(S/N=10)为0.05～0.5 mg/kg。在0.10～10 mg/kg加标水平下的回收率为83%～106%,相对标准偏差(RSD,n=6)为2.9%～5.5%。采用该方法研究了华南地区不同食品及包装材料中邻苯二甲酸酯含量的分布情况,并对其来源进行了探讨。

A sensitive method for the simultaneous determination of 21 phthalate acid esters （PAEs） in foods by gas chromatography - mass spectrometry（ GC -MS） was firstly proposed. Different separation and purification methods were selected according to the types of food, and the chromatographic conditions were optimized. Qualitative detection and confirmation were acquired by the extraction of characteristic ions, and the interferences due to the complex matrixes were effectively eliminated, thus avoiding the possibility of false positive results. The mass spectrometric fragmentation rule of PAEs was also discussed in detail. The calibration curves of 21 compounds were linear in the range of 0. 1 - 100 mg/L with correlation coefficients not less than 0. 999 2. The quantitative limits （LOQs, S/N = 10） ranged from 0.05 mg/kg to 0.5 mg/kg. The average spiked recoveries were in the range of 83% -106% at spiked levels of 0. 10 -10 mg/kg with relative standard deviations（ RS- Ds, n = 6） of 2.9% - 5.5%. The method was successfully applied in the investigation of the PAEs distribution in foods and food packaging material of South China area, and the source of PAEs was also discussed in detail.