气相色谱法测定蔬菜中三碘苯甲酸残留量-食品科学.PDF

178 2010, Vol. 31, No. 12 食品科学 ※分析检测 周艳明，付 婷，胡 睿 (沈阳农业大学分析测试中心，辽宁沈阳 110161) ：建立三碘苯甲酸残留量的气相色谱测定方法，选取西红柿等6 种基质，样品经0.1mol/L 盐酸酸化，以二 氯甲烷为提取剂，超声波提取，用三甲基硅重氮甲烷进行甲酯化，经弗罗里硅土固相萃取柱净化后上机测定，采 用电子捕获检测器测定，保留时间定性，外标法定量。并对该方法的灵敏度、准确度和精密度进行实验，三碘 苯甲酸的最低检出限可达0.001mg/kg ，各水平的添加回收率为70%～95.7% 。该方法可靠、灵敏、简便可行，可 为制定国家标准分析方法提供参考。 ：三碘苯甲酸；蔬菜；衍生反应；S P E 净化；气相色谱 GC Determination of 2,3,5-Triiodobenzoic Acid Residue in Vegetables ZHOU Yan-ming ，FU Ting ，HU Rui (Analysis and Testing Center, Shenyang Agricultural University, Shenyang 110161, China) Abstract ：A gas chromatographic (GC) method was developed for the determination of 2,3,5-triiodobenzoic acid (TIBA) in vegetables. The main steps in sample preparation prior to the injection of processed samples into a GC system equipped with an electron capture detector consisted of acidification with 0.1 mol/L hydrochloric acid, extraction with methylene dichloride under ultrasonic assistance, methylation with trimethylsilyl diazomethane and clean-up on a florisil solid phase extraction (SPE). Retention time was used for qualification and external standard method for quantification. Some figures of merit the method developed including sensitivity, accuracy and precision were evaluated. This method exhibited a limit of detection of 0.001 mg/kg for TIBA. Mean recoveries for the analyte in 6 vegetable matrices ranged from 70% to 95.7%. These results suggest that this method is reliable, sensitive, simple and convenient and can provide useful references for the establishment of a national standard method for the determination of TIBA. Key words ：2,3,5-triiodobenzoic acid ；vegetables ；derivation ；SPE purification；gas chromatography 中图分类号：TS207.7