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离子色谱-电感耦合等离子体质谱法检测食品中磷酸盐形态及含量

Determination the phosphate form and content in food by ion chromatography-inductively coupled plasma mass spectrometry
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摘要 目的 建立离子色谱-电感耦合等离子体质谱法检测食品中正磷酸盐、焦磷酸盐、三偏磷酸盐、三聚磷酸盐和六偏磷酸盐不同形态及其含量的方法。方法 样品通过超声辅助提取-三氯甲烷沉淀-固相萃取净化前处理方式,采用离子色谱-电感耦合等离子体质谱法测定,以氧气为反应气体消除质谱干扰,以外标法进行定量分析。结果 5种形态的磷酸盐在12 min内实现基线分离,在0~20 mg/L范围内呈良好线性关系,相关系数(r)均大于等于0.9997,平均回收率为87.7%~107.0%,检出限为0.15~1.79 mg/kg,相对标准偏差为1.12%~4.95%。应用本方法分析市售肉制品、米粉制品以及婴幼儿配方食品,所有样品中磷酸盐含量均符合GB 2760—2024《食品安全国家标准食品添加剂使用标准》的限量要求,且未检出非许可形态磷酸盐。结论 该方法准确高效,检出限低,适用于食品中5种形态磷酸盐的分离检测。本研究为食品中磷酸盐形态检测与风险评估提供技术支持,对磷酸盐食品添加剂精准靶向监管具有实践意义。 Objective To establish a method for the detection of different forms and their content of orthophosphate,pyrophosphate,triaphosphate,tripolyphosphate and hexametaphosphate in food by ion chromatography-inductively coupled plasma mass spectrometry.Methods The samples were treated by ultrasonic-assisted extraction-trichloromethane precipitation-solid-phase extraction purification pretreatment.The determination was carried out by ion chromatography-inductively coupled plasma mass spectrometry.Oxygen was used as the reaction gas to eliminate mass spectrometry interference,and quantitative analysis was conducted by the external standard method.Results The 5 kinds of forms of phosphates achieved baseline separation within 12 minutes,demonstrating good linearity in the range of 0–20 mg/L,with correlation coefficients(r)all greater than or equal to 0.9997.The average recovery rates were 87.7%–107.0%,the limits of detection were 0.15–1.79 mg/kg,and the relative standard deviation was 1.12%–4.95%.This method was applied to analyze commercially available meat products,rice flour products and infant formula foods.The phosphate content in all samples complied with the limits specified in GB 2760—2024 National food safety standard—Standards for the use of food additives,and no non-permitted forms of phosphates were detected.Conclusion The method is accurate and efficient with low detection limit,and is suitable for the separation and detection of 5 kinds of phosphate species in food.This study provides technical support for phosphate morphological detection and risk assessment in food,and has practical significance for precise targeted supervision of phosphate food additives.
作者 陈景周 梁志森 陈思敏 陈京成 钟新林 CHEN Jing-Zhou;LIANG Zhi-Sen;CHEN Si-Min;CHEN Jing-Cheng;ZHONG Xin-Lin(Guangzhou Inspection Testing and Certification Group Company Limited,National Quality Inspection and Testing Center for Processed Foods(Guangdong),Guangzhou 511400,China;Prin-cen Scientific Limited of Guangzhou,Guangzhou 510700,China)
出处 《食品安全质量检测学报》 2025年第17期61-67,共7页 Journal of Food Safety and Quality
基金 广州市市场监督管理局科技项目(2023KJ50)。
关键词 离子色谱-电感耦合等离子体质谱法 磷酸盐形态 定量分析 ion chromatography-inductively coupled plasma mass spectrometry phosphate species quantitative analysis
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