气相色谱-质谱法检测蔬菜中3种主要塑化剂含量

Determination of 3 main plasticizers in vegetables by gas chromatography-mass spectrometry

目的建立气相色谱-质谱法检测蔬菜中邻苯二甲酸二(2-乙基己基)酯(Di(2-ethylhexyl)phthalate,DEHP)、邻苯二甲酸二异丁酯(diisobutyl phthalate, DIBP)以及邻苯二甲酸二丁酯(dibutyl phthalate, DBP)3种主要塑化剂的含量。方法样品经正己烷超声提取后,经Ttx-5MS(30.0 m×0.25 mm×0.25μm)色谱柱分离,进样口温度为260℃;载气流速为1.0 mL/min,柱箱程序升温,外标法定量检测。结果在0.025~0.5μg/mL浓度范围内3种塑化剂的线性关系良好(r>0.999),检出限分别为0.0048、0.0080、0.015μg/mL,加标回收率为103.68%~118.65%,相对标准偏差在1.16%~5.23%,满足定量分析要求。结论本方法简单,快速,适用于不同蔬菜中3种塑化剂的定量分析,且部分塑化剂类化学污染物在叶菜类蔬菜中存在污染积累效应。

Objective To establish a method for the determination the content of 3 main plasticizers of Di(2-ethylhexyl) phthalate(DEHP), diisobutyl phthalate(DIBP) and dibutyl phthalate(DBP) in vegetables by gas chromatography-mass spectrometry. Methods The sample was ultrasonically extracted by n-hexane and separated by Ttx-5 MS(30.0 m×0.25 mm×0.25 μm) column. The inlet temperature was 260 ℃. The carrier gas flow rate was 1.0 mL/min, the temperature was programmed in the column box, and the content was quantitative detected by external standard method. Results The linear relationship of the 3 plasticizers was good in the concentration range of 0.025~0.5 μg/mL(r>0.999), and the limits of detection were 0.0048, 0.0080, 0.015 μg/mL, respectively. The standard recoveries were 103.68%-118.65%, with the relative standard deviations were 1.16%-5.23%, which met the requirements of quantitative analysis. Conclusion The method is simple and rapid, and is suitable for quantitative analysis of three plasticizers in different vegetables, and some plasticizer chemical pollutants have a pollution accumulation effect in leafy vegetables.