气相色谱-质谱法测定小麦粉中苯甲酸含量  

Determination of benzoic acid content in wheat flour by gas chromatography-mass spectrometry

作　　者：周宏霞 张梅超 王秀丽 燕娜娜 ZHOU Hong-xia;ZHANG Mei-chao;WANG Xiu-li;YAN Na-na(Weihai Institute for Food and Drug Inspection and Testing,Weihai 264210,China;Rongcheng Inspection and Testing Center,Rongcheng 264300,China)

机构地区：[1]威海市食品药品检验检测研究院,山东威海264210 [2]荣成市检验检测中心,山东荣成264300

出　　处：《粮食与饲料工业》2024年第5期80-83,共4页Cereal & Feed Industry

摘　　要：建立了一种气相色谱-串联三重四级杆质谱的苯甲酸添加剂测定方法,并对该检测方法的参数进行了优化。试验结果表明:(1)当以酸性石油醚作为提取试剂时,在提取固液比为1∶8,超声提取时间为50 min条件下,苯甲酸的提取率最高;(2)在最优参数条件下,苯甲酸的检出限和定量限分别为0.5 mg/kg和1.5 mg/kg,在1~100μg/mL的浓度范围内表现出良好的线性关系,且相关系数R 2大于0.999;在1、10、20 mg/kg加标水平下,苯甲酸回收率在91.7%~107.6%范围内,其中在10 mg/kg加标水平下的相对标准偏差(RSD)为0.9%。综上,该检测方法简单、快捷和准确,可用于小麦粉中添加剂残留量的测定。This experiment establishes a gas chromatography-tandem triple quadrupole mass spectrometry method for determining benzoic acid additives,and optimizes the parameters of the proposed method.The experimental results show that:(1)the highest benzoic acid extraction rate is achieved when acidic petroleum ether is used as the extracting solvent,solid-to-liquid ratio is 1∶8,and ultrasound extraction lasts 50 min;(2)under the optimal parametric conditions,the benzoic acid detection limit and quantitative limit are 0.5 mg/kg and 1.5 mg/kg,respectively;good linear relationship is seen in 1-100μg/mL concentration range and the corresponding correlation coefficient R 2 is over 0.999;when spiked at 1 mg/kg,10 mg/kg and 20 mg/kg,benzoic acid recovery rate ranges within 91.7%-107.6%and the relative standard deviation(RSD)is 0.9%at 10 mg/kg spiking level.To sum up,the method proposed in this paper is simple,convenient and precise,which warrants its applicability to the determination of benzoic acid residue in wheat flour.

关 键 词：小麦粉 苯甲酸 添加剂 气相色谱 三重四级杆质谱 石油醚 提取率 

分 类 号：TS211.7[轻工技术与工程—粮食、油脂及植物蛋白工程]