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气相色谱-质谱法测定小麦粉中苯甲酸含量

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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1~100 μg/mL的浓度范围内表现出良好的线性关系,且相关系数R2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.
Determination of benzoic acid content in wheat flour by gas chromatography-mass spectrometry
This experiment establishes a gas chromatography-tandem triple quadrupole mass spectrometry method for deter-mining 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 1-100 μg/mL concentration range and the corresponding correlation coefficient R2 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 lev-el.To sum up,the method proposed in this paper is simple,convenient and precise,which warrants its applicability to the deter-mination of benzoic acid residue in wheat flour.

wheat flourbenzoic acidadditivesgas chromatographytriple quadrupole mass spectrometrypetroleum etherextraction rate

周宏霞、张梅超、王秀丽、燕娜娜

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威海市食品药品检验检测研究院,山东威海 264210

荣成市检验检测中心,山东荣成 264300

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

2024

粮食与饲料工业
国家粮食储备局 武汉科学研究设计院

粮食与饲料工业

CSTPCD
影响因子:0.513
ISSN:1003-6202
年,卷(期):2024.(5)