碱液提取离子色谱法测定水产品中多聚磷酸盐的研究
详细信息Determination of polyphosphates in aquatic products by alkali liquor extraction-ion chromatography
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摘要: 建立了碱液提取水产品中多聚磷酸盐并同时测定焦磷酸盐、三聚磷酸盐和六偏磷酸盐的离子色谱法。以3mol/L NaOH溶液为提取液,回收率达90%以上,有效阻断了多聚磷酸盐的水解。在AS11-HC阴离子色谱柱上,焦磷酸盐、三聚磷酸盐和六偏磷酸盐分离度良好,在质量浓度为1.0～100.0mg/mL的范围内,其浓度与峰面积成良好的线性关系。在优化的色谱条件下,三种多聚磷酸盐的测定低限分别为:焦磷酸3.0mg/kg,三聚磷酸盐为3.0mg/kg,六偏磷酸盐为10.0mg/kg。以鲢鱼为空白样,添加三个浓度（1.0、10.0、50.0mg/mL）进行精密度和回收率实验,RSD在4.0%以下,回收率在95%～100%。Abstract: Established a method for extracting polyphosphates from aquatic products and simultaneously determined pyrophosphate, tripolyphosphate, hexametaphosphate by ion chromatography.Using 3mol/L NaOH as extraction solution could inhibit hydrolysis of polyphosphates effectively, recovery rate was more than 90%.In AS11-HC anionic chromatography column, the separation degree of pyrophosphate, tripolyphosphate, hexametaphosphate were fine.The concentration and peak area exhibited linearity in the range from 1.0～100.0mg/mL.In the condition of optimization of chromatographic, the low determination limits of pyrophosphate, tirpolyphosphate and hexametaphosphate were 3.0mg/kg, 3.0mg/kg and 10.0mg/kg respectively.Using silver carp as blank sample, added three concentrations (1.0, 10.0, 50.0mg/mL) for accuracy and recovery rates tests, the RSD was below 4.0% and the recovery rates were in the range of 95%～100%.
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