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    高效液相色谱法同时测定酱腌菜中5种添加剂

    HPLC Simultaneous Determination 5 Kinds of Additives in Pickles

    • 摘要: 提出了高效液相色谱法同时测定酱腌菜中5种添加剂安赛蜜、糖精钠、苯甲酸、山梨酸和脱氢乙酸的含量。样品采用0.02 mol·L-1氢氧化钠溶液超声提取后,采用乙酸铅和硫酸钠沉淀样品,经0.45 μm滤膜过滤,滤液供高效液相色谱仪测定。采用Agilent C18色谱柱(250 mm×4.6 mm,5 μm)分离,用甲醇-0.02 mol·L-1磷酸二氢钾(25+75)混合溶液为流动相洗脱,用二极管阵列检测器在波长225 nm处测定。5种添加剂的质量浓度均在5~100 mg·L-1范围内与峰面积呈线性关系;检出限(2S/N)在1~2 mg·L-1之间。方法的回收率在85.6%~105.8%之间;测定值的相对标准偏差(n=6)均小于5.0%。

       

      Abstract: HPLC was applied to the determination of 5 kinds of additives, including acesulfame potassium, saccharin sodium, benzoic acid, sorbic acid and dehydroaectic acid in pickles. The sample was extracted ultrasonically with 0.02 mol·L-1 NaOH solution and precipitated with Pb(CH3COO)2-Na2SO4 . After filtering on 0.45 μm filtering membrane, the filtrate was used for HPLC analysis. The Agilent C18 chromatographic column (250 mm×4.6 mm, 5 μm)was used for separation and a mixture of methanol and 0.02 mol·L-1 KH2PO4 solution (25+75) was used as the mobile phase. Diode array detector at the wavelengths of 225 nm was adopted in the determination. Linear relationships between values of peak area and mass concentration of the 5 additives were obtained in the range of 5-100 mg·L-1, with detection limit (2S/N) in the range of 1-2 mg·L-1. Values of recovery of the method found were in the range of 85.6%-105.8%, with RSD′s (n=6) less than 5.0%.

       

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