酸水解法联合离子色谱测定食品中总磷酸盐含量的应用研究  

Application of Acid Hydrolysis Combined with Ion Chromatography in The Determination of Total Phosphate in Foods

作　　者：梁敏 黄媛 唐雯 陈言凯 江凤玲 李燕妹 LIANG Min;HUANG Yuan;TANG Wen;CHEN Yankai;JIANG Fengling;LI Yanmei(Fujian Inspection and Research Institute for Product Quality,National Quality Supervision and Testing Center for Processed Food,Fuzhou 350001,China)

机构地区：[1]福建省产品质量检验研究院,国家加工食品质量监督检验中心,福建福州350001

出　　处：《食品科技》2023年第9期253-258,共6页Food Science and Technology

基　　金：食品安全国家标准修订项目(spaq-2020-041);福建省产品质量检验研究院科技项目(KY202219A)。

摘　　要：研究旨在建立酸水解法联合离子色谱测定食品中总磷酸盐含量。方法采用硝酸高温水解,将样品提取溶液中焦磷酸根(P_(2)O_(7)^(4-))、三偏磷酸根((PO_(3))_(3)^(3-))、三聚磷酸根(P_(3)O_(10)^(5-))、六偏磷酸根(P_(6)O_(18)^(6-))等多种磷酸盐水解转化为正磷酸根(PO_(4)^(3-)),后注入离子色谱仪,电导检测器检测总磷酸盐含量(以PO_(4)^(3-)计)。实验对提取路线及色谱条件进行了优化,确定了最佳检测方法,并对所建立方法进行方法学评价。结果显示,正磷酸盐在0.05~20.0μg/m L浓度范围内线性良好,相关系数r^(2)大于0.999,检出限为10 mg/kg,定量限为100 mg/kg,乳制品、肉制品等不同基质样品加标回收率在87.2%~107%。该方法前处理步骤简便、不易受复杂基质影响,准确性、灵敏度高,分析速度快,适用于食品中总磷酸盐含量的测定。A method for the determination of total phosphate in foods was developed by using acid hydrolysis combined with ion chromatography.The sample were extracted with nitric acid hydrolysis at boiling water bath,that turned the polyphosphate into orthophosphate(PO_(4)^(3-)),which included pyrophosphate(P_(2)O_(7)^(4-)),trimetaphosphate((PO_(3))_(3)^(3-)),tripolyphosphate(P_(3)O_(10)^(5-)),hexametaphosphate(P_(6)O_(18)^(6-)).The extraction were injected into ion chromatography with suppressed conductivity detection for the determination of total phosphate(calculated in PO_(4)^(3-)).The method was confirmed after optimized of the extraction and chromatographic conditions.The methodological investigation results showed that the corresponding linear range(0.05–20μg/mL)for analysis exhibited a good linearity(r^(2)≥0.999),the detection of limits(LOD)was 10 mg/kg,quantitation of limits(LOQ)was 100 mg/kg,the spiked recoveries of meat products,dairy products,etc,were obtained over 87.2%–107%.The method exhibits high accuracy and sensitivity,with simple pretreatment procedure and no matrix pollution,which was suitable for the detdction of total phosphate in food.

关 键 词：酸水解法 离子色谱 总磷酸盐 食品 

分 类 号：TS207.5[轻工技术与工程—食品科学]