柱前衍生高效液相色谱法检测水产品中甲醛的含量

Determination of formaldehyde in aquatic products by high performance liquid chromatography with precolumn derivatization

中文关键词:  甲醛  水产品  柱前衍生  高效液相色谱法

英文关键词:formaldehyde  aquatic product  precolumn derivatization  high performance liquid chromatography

中文摘要:

      目的 建立柱前衍生高效液相色谱法检测水产品中甲醛含量。方法 样品经绞碎匀浆后, 经2, 4-二硝基苯肼-乙酸钠缓冲液衍生液(1:1, V:V)于60 ℃衍生1 h, 冰浴冷却后的衍生物直接上高效液相色谱检测, 以ODS-C18柱子为分离柱, 甲醇-水(70:30, V:V)为流动相等度洗脱, 二极管阵列检测器在365 nm波长处检测, 外标法定量。结果 甲醛在0~10 mg/L浓度范围内线性关系良好, 线性相关系数为0.9994, 方法检出限为0.5 mg/kg。空白样品在 1.0、5.0和20.0 mg/kg添加水平下, 回收率在88.2%~95.3%之间, RSD在0.75%~1.82%之间。对水产品9种样品中的甲醛进行了测定, 其中6个样品检出甲醛, 含量范围为1.51~64.04 mg/kg。结论 该方法简便、灵敏、准确, 可适用于水产品中甲醛含量的分析。

英文摘要:

      Objective To establish a method for the determination of formaldehyde in aquatic products by high performance liquid chromatography with precolumn derivatization. Methods After homogenation and homogeneity, samples were derivatized with 2, 4-dinitrobenzene hydrazine derivative-sodium acetate buffer (1:1, V:V) at 60 ℃ for 1 h. After ice bath cooling, the derivatives were determined by high performance liquid chromatography (HPLC) using ODS-C18 column for separation with methanol and water (70:30, V:V) as the mobile phase for isocratic elution, and then detected by diode array detector at 365 nm wavelength with external standard method for quantification. Results Formaldehyde had a good linear relationship in the range of 0~10 mg/L with correlation coefficient of 0.9994, and the limit of detection was 0.5 mg/kg. The recoveries spiked at 3 levels of 1.0, 5.0 and 20.0 mg/kg were 88.2%~95.3% with RSD of 0.75% ~ 1.82%. Nine aquatic products were determined, and 6 samples were detected, the content range of formaldehyde were 1.51~64.04 mg/kg. Conclusion The method is simple, sensitive and accurate, which can be applied for the analysis of formaldehyde in aquatic products.