气相色谱-氮磷检测器法测定小麦粉及其制品与小麦粉添加剂中的乙酰氧肟酸  

Determination of acetohydroxamic acid in wheat flour and its products and wheat flour additives by GC-NPD

作　　者：宁亚萍 武文凯 石璐 刘璐 李彤辉 谷瑞丽 NING Ya-ping;WU Wen-kai;SHI Lu;LIU Lu;LI Tong-hui;GU Rui-li(Henan Institute of Food and Salt Industry Inspection Technology,Zhengzhou 450003,Henan,China;Key Laboratory of Food Safety Quick Testing and Smart Supervision Technology for State Market Regulation,Zhengzhou 450003,Henan,China)

机构地区：[1]河南省食品和盐业检验技术研究院,河南郑州450003 [2]国家市场监管重点实验室(食品安全快速检测与智慧监管技术),河南郑州450003

出　　处：《粮食与油脂》2024年第3期148-153,共6页Cereals & Oils

基　　金：国家市场监督管理总局研究委托任务资助;河南省科技攻关项目(212102410010);国家自然科学青年基金资助项目(31901820)。

摘　　要：建立了气相色谱-氮磷检测器法测定小麦粉及其制品与小麦粉添加剂中非法添加物乙酰氧肟酸(AHA)的分析方法。以小麦粉、小麦粉添加剂、面皮、面条、馒头为研究基质,优化了色谱条件,并通过向5种空白基质进行加标回收实验优化前处理方法。样品经无水乙醇超声和涡旋振荡提取,高速离心、过滤,采用DB-WAX(60 m×0.32 mm,0.25μm)色谱柱分离,外标法定量。结果表明:AHA溶剂和基质标准曲线在0.60~10.00μg/mL范围内线性关系良好,相关系数均大于0.998,检出限为2 mg/kg,定量限为6 mg/kg;加标回收率为86.19%~109.22%,相对标准偏差(n=6)为1.47%~7.89%。方法适用于小麦粉及其制品与小麦粉添加剂中AHA的测定。An analytical method of illegal additives acetohydroxamic acid(AHA)in wheat flour and its products and wheat flour additives was developed by gas chromatography-nitrogen phosphorus detector method.Wheat flour,wheat flour additive,flour crust,noodles and steamed bread were selected as the research matrix.The chromatographic conditions were optimized,and the pretreatment method was optimized by spiked recovery tests with adding standard material to five kinds of blank matrices.Samples were extracted with anhydrous ethanol by ultrasonic and vortex oscillation,followed by high-speed centrifugation and filtration.DB-WAX(60 m×0.32 mm,0.25μm)was used to extract the sample chromatographic column separation,and quantified by external standard method.The results showed that the sol-vent and matrix standard curves of AHA had a good linear relationship in the mass concentration range of 0.60-10.00μg/mL,with correlation coefficients of higher than 0.998.The limits of detection was 2 mg/kg,and the limit of quantification was 6 mg/kg.The recovery rate of spiking was 86.19%-109.22%,and the relative standard deviation(n=6)was 1.47%-7.89%.The method could be used for the determination of AHA in wheat flour and its products and wheat flour additives.

关 键 词：小麦粉 乙酰氧肟酸 气相色谱-氮磷检测器法 

分 类 号：TS211.7[轻工技术与工程—粮食、油脂及植物蛋白工程]