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    衍生液提取-高效液相色谱法测定食品中甲醛

    HPLC Determination of Formaldehyde in Foodstuffs by Extraction with Derivative Solution

    • 摘要: 提出了高效液相色谱法测定了几种食品中甲醛含量。以衍生液2,4-二硝基苯肼乙腈溶液-pH 5的磷酸盐缓冲溶液(1+1)的混合溶液为提取剂对样品进行提取,以Agilent C18色谱柱(4.6 mm×250 mm,5 μm)为固定相,以甲醇-水(70+30)溶液为流动相分离。甲醛的测定下限(10S/N)为5.0 mg·kg-1。以鲜香菇、鲜鱿鱼、奶粉和面粉样品为基体,分别添加5.0,10.0,20.0 mg·kg-1甲醛标准溶液,回收率在73.3%~97.7%之间,相对标准偏差(n=6)在1.4%~5.0%之间。

       

      Abstract: HPLC was applied to the determination of formaldehyde in some foodstuffs. The formaldehyde in sample was extract with a mixture of 2,4-dinitro-phenylhydazine (dissolved in acetonitrile) and phosphate buffer solution of pH 5 (1+1) as derivatizing solution, and separated on Agilent C18 column (4.6 mm×250 mm, 5 μm). A mixture of methanol and water mixed in the ratio of 70 to 30 (by volume) was used as mobile phase. Values of limit of determination (10S/N) found was 5.0 mg·kg-1. Using samples of fresh mushroom, fresh squid, milk powder and flour as matrixes, tests for recovery were made by standard addition method at 3 concentration levels of 5.0, 10.0 and 20.0 mg·kg-1, and the results obtained were in the range of 73.3%-97.7%, with values of RSD′s (n=6) in the range of 1.4%-5.0%.

       

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