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投稿时间：2025-02-11
投稿时间：2025-02-11
中文摘要: 建立顶空固相微萃取-气相色谱-质谱法测定粮谷中溴甲烷含量的分析方法。采用固相微萃取技术，从样品中吸附溴甲烷，通过顶空富集，用气相色谱-质谱联用仪进行分离和定性分析，外标法定量。结果表明，溴甲烷在0.01～1.00 μg/mL浓度范围内有良好的线性关系，相关系数（R2）大于0.999，方法检出限为0.003 mg/kg，定量限为0.01 mg/kg；稻谷、小麦、玉米、黑米和面粉在3个添加水平（0.01、0.05、0.10 mg/kg）下的加标回收率为84.5%～97.7%，相对标准偏差（relative standard deviations，RSD）为4.33%～7.64%。该方法样品处理简单快速，灵敏度高、重复性好，可用于粮谷类样品中溴甲烷的批量定量测定。
Abstract:A method for the determination of methyl bromide residues in cereals was established based on headspace solid-phase microextraction coupled with gas chromatography-mass spectrometry.Methyl bromide was obtained from the sample by solid-phase microextraction,separated and qualitatively analyzed by gas chromatography-mass spectrometry,and quantitatively determined by the external standard method.The results showed that methyl bromide showed good linear relationship between peak area and concentration within the range of 0.01-1.00 μg/mL,with R2 greater than 0.999.The established method showed the limit of detection being 0.003 mg/kg and the limit of quantitation being 0.01 mg/kg.The average recovery rates of methyl bromide were in the range of 84.5% to 97.7% at three spiked levels of 0.01,0.05 mg/kg,and 0.10 mg/kg in rice,wheat,maize,black rice,and flour,with the relative standard deviations in the range of 4.33% to 7.64%.The method was simple and fast in sample processing,with high sensitivity and good repeatability,and thus can be used for the quantitative determination of methyl bromide in cereals.
keywords: headspace solid-phase microextraction gas chromatography-mass spectrometry solid-phase microextraction fiber cereals methyl bromide
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