柱前衍生高效液相色谱法检测水产品中甲醛的含量
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。
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.
标题：柱前衍生高效液相色谱法检测水产品中甲醛的含量
英文标题：Determination of formaldehyde in aquatic products by high performance liquid chromatography with precolumn derivatization
作者：
唐穂平 广东产品质量监督检验研究院
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,
发表日期：2016-06-02
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