水产品中甲醛的柱后衍生-高效液相色谱测定法

Determination of formaldehyde in aquatic products by high performance liquid chromatography with post-column derivatization

目的建立一种水产品中甲醛柱后衍生-高效液相色谱荧光检测的分析方法。方法样品经过三氯乙酸超声提取后,过滤进样,经反相ODS-C_(18)柱分离,在衍生池温度为100℃条件下,与0.05 mol/L乙酰丙酮、0.81 mol/L乙酸铵进行衍生,荧光检测器检测,外标法定量。结果甲醛质量浓度在0.025~10.0 mg/L范围内呈良好线性,相关系数为0.999 3,方法检出限为0.10 mg/kg,定量限为0.25 mg/kg,加标回收率为84%~95%。与水蒸气蒸馏-分光光度法比较,差异无统计学意义。结论方法前处理简单,干扰少,检出限低,适用于水产品中甲醛含量的测定。

[Objective]To develop a method for determination of formaldehyde in aquatic products by high performance liquid chromatography with post-column derivatization and fluorescence detection. [Methods] After pre-treated by trichloroacetic acid combined with ultra-sonic extraction and filtration,the samples was injected and analyzed by high performance liquid chromatography with an ODS-C18 column and a fluorescence detector. As the temperature of the derivatization pool was 100 ℃,0.05 mol/L acetylacetone and 0.81 mol/L ammonium acetate were the post column derivatization reagents. The fluorescence detector was applied in detection,and the quantitative analysis was performed according to the external standard method.[Results] Under optimal experimental conditions,good linearity was observed in the range of 0.025-10.0 mg/L with a correlation coefficient of 0.999 3. The limit of detection was 0.10 mg/kg. The limit of quantitation was 0.25 mg/kg. The recoveries of formaldehyde were in the range of 84%-95%.Compared with steam distillation colorimetric method,there was no significant difference. [Conclusion] The method has the advantages of simple pre-treatment,less interference,and lower detection limit,and it is suitable for analysis of formaldehyde in aquatic products.