高级检索

    毛细管柱-气相色谱法测定食品中脱氢乙酸

    GC Determination of Dehydroacetic Acid in Food with Capillary Column

    • 摘要: 应用毛细管柱-气相色谱法测定了食品中脱氢乙酸(DHA)。对含水较少的样品,取5.000 g样品,用含有经乙腈饱和的氯化钠溶液10 mL,氯化钠4~5 g,冰乙酸200 μL及乙腈5 mL的溶液提取其中的DHA。经剧烈振摇及离心分离后,取上层清液2.00 mL,加入50 g·L-1苯甲酸溶液80 μL及无水硫酸镁300 mg,离心分离。苯甲酸作为测定物的保护剂加入。对含水较多的样品,取10.000 g样品,用含有冰乙酸250 μL,乙腈10 mL,氯化钠1 g及无水硫酸镁4 g的溶液进行提取并离心分离。取2.00 mL上层清液按上述方法处理,最终所得上层清液用于气相色谱分析。测定中采用HP-5毛细管柱及火焰离子化检测器,测得DHA的线性范围在2.5~1 000 mg·L-1之间,其测定下限(10S/N)为0.005 g·kg-1。用3种不同的食品样,在4个浓度水平上进行回收及精密度试验,测得回收率在84.3%~107.9%之间,相对标准偏差(n=6)在2.6%~4.5%之间。

       

      Abstract: Gas chromatography with capillary column was applied to the determination of dehydroacetic acid (DHA) in food. For samples containing less moisture, DHA was separated from 5.000 g of sample by extraction from a solution containing 10 mL of sat′d NaCl solution (saturated also with acetonitrile), 4-5 g of NaCl, 200 μL of glacial acetic acid and 5 mL of acetonitrile. After vigorous shaking and centrifugation, 2.00 mL of the supernatant were taken and treated with 80 μL of 50 g·L-1 benzoic acid solution and 300 mg of anhydrous MgSO4 by centrifugation. Benzoic acid was added as a protectant for the analyte. For wet samples, 10.000 g of the sample were taken and the extraction was carried out in a solution containing 250 μL of glacial acetic acid, 10 mL of acetonitrile, 1 g of NaCl and 4 g of anhydrous MgSO4. After shaking and centrifugation, 2.00 mL of the supernatant were taken and treated further as described above. The supernatant finally obtained was used for the GC analysis. HP-5 capillary column and flame ionization detector were adopted in the determination. Linearity range for DHA was found between 2.5-1 000 mg·L-1 with the lower limit of determination (10S/N) of 0.005 g·kg-1. Recovery and precision were tested on 3 kinds of food at 4 concentration levels, giving results of recovery ranged from 84.3% to 107.9% and RSD′s (n=6) ranged from 2.6% to 4.5%.

       

    /

    返回文章
    返回