GC-MS法测定塑料中对特辛基苯酚残留量

Plastic Products of Octyl Phenol Determination of the Residues GC-MS Method

建立了用气相色谱-质谱法(GC-MS)检测塑料中对特辛基苯酚残留量的方法。试样经低温冷冻粉碎,丙酮溶解,微波萃取,提取液经浓缩定容进入DB-5MS石英毛细管色谱柱(30 m×0.25 mm,0.25μm)分离,采用GC-MS选择离子检测,外标法定量。结果表明,在(0.1~2.0)mg/L范围内,相关系数r大于0.99,方法检出限为0.221μg/L,定量限为0.737μg/L。当添加对特辛基苯酚含量为0.1、0.2、0.5、1.0、2.0 mg/L时,加标回收率在85.7%~105.0%之间,其RSD数为2.1%~3.3%(n=6)。该方法具有方法科学、准确、实用性强、样品处理简单、分析速度快、选择性和重复性好、便于高通量使用等特点。适用于塑料中对特辛基苯酚残留量的检测,易于推广应用。

A method for the determination of texylphenol residues in plastic products by gas chromatography-mass spectrometry （GC-MS） was established. The samples were separated by cryopreservation, acetone dissolution, microwave extraction and concentrated solution. The samples were separated into DB-5 MS quartz capillary column（30 m × 0. 25 mm ,0.25 μm）. The samples were separated by GC-MS and quantified by external standard method. The results showed that the correlation coefficient r was more than 0.99,in the range of（0.1 -2.0） mg/L,the detection limit was 0. 221 μg/L and the limit of quantification was 0. 737μg/L. When the addition of p-octylphenol was 0. 1,0.2,0.5,1.0 and 2.0 mg/L, the recoveries ranged from 85.7% - 105.0% , and the RSD was 2. 1% - 3.3% （n = 6）. The method had the advantages of scientific method, accurate and practicality, simple sample processing, fast analysis speed, selectivity and repeatability, and been convenient for high throughput. It is suitable for the detection of texylphenol residues in plastic products and is easy to popularize and apply.