农用棚膜中邻苯二甲酸酯的测定

The Determination of Phthalate Plasticizers in Shed Film

采用微波辅助提取和常规的气相色谱分离方法,对农用棚膜中6种邻苯二甲酸酯类（PAEs）增塑剂的检测进行了实验研究。选用正己烷作为提取剂,利用单因素和正交实验对提取条件进行了优化,棚膜样品破碎至1.0 cm×2.0 cm,料液比（m L/g）1∶50,微波功率400 W,萃取时间8 min能获得最佳提取效果。采用气相色谱法,在DB-5MS（30 m×0.25 mm×0.25μm）色谱柱上利用程序升温对样品进行分离,氢火焰离子化检测器进行检测。该方法在2.0~1 000 mg/L范围具有良好线性关系,相关系数均大于0.999,检测限0.15~0.60 mg/kg,符合国家限量标准,样品加标回收率85.4%~110.7%,相对标准偏差0.61%~7.47%。该方法操作简单,灵敏度高,不仅可以满足农用棚膜中邻苯二甲酸酯类化合物的分析检测,并可应用于本科生仪器分析实验教学。

A method was established for the determination of 6 phthalate plasticizers in shed film by microwave assisted extraction-gas chromatography. Using n-hexane as the extraction solvent,the extraction conditions were optimized by single factor and orthogonal analysis. The optimum extraction conditions were 1. 0 cm × 2. 0 cm of the fragmentation film sample,1 ∶ 50 of material and liquid ratio,400 W extracted power,8min extraction time. The samples were separated by gas chromatography（ GC） on a DB-5MS column（ 30 m × 0. 25 mm × 0. 25 μm）,and detected by flame ionization detector. The results showed that all the correlation coefficients were over 0. 999 in the range of 2. 0- 1 000 mg / L,the recoveries were 85. 4%- 110. 7%,the relative standard deviations were 0. 61%- 7. 47%,and the detection limits were 0. 15- 0. 60 mg / kg- 1,respectively. This method was simple and sensitive,and was suitable for the determination of phthalate plasticizers in shed film and the comprehensive experiment teaching.