顶空气相色谱-质谱法测定白酒中的氰化物含量

Determination of cyanide in liquor by headspace gas chromatography-mass spectrometry

中文关键词:  氰化物  白酒  顶空气相色谱-质谱法

英文关键词:cyanide  liquor  headspace gas chromatography-mass spectrometry

中文摘要:

      目的 建立顶空气相色谱-质谱法测定白酒中的氰化物含量的方法。方法 优化顶空平衡温度、时间、pH值、氯胺T加入量, 以顶空进样器注入气相色谱质谱联用仪进行分离检测, 并应用该方法对市售的米香型、清香型、豉香型和浓香型4种香型的白酒进行加标后检测。结果 白酒中的氰化物在0.001~0.2 mg/L线性范围内线性关系良好, 回归系数r2=0.9996, 检出限为0.01 mg/L(S/N≥3), 定量限为0.03 mg/L(S/N≥10), 加标回收率在71.6%~116.2%之间, 相对标准偏差(relative standard deviation, RSD)为1.3%(n=6)。结论 该方法简便快捷, 结果准确度高, 相比国标中的气相色谱法, 明显缩短了检测周期, 提高了检测效率, 可用于白酒中氰化物含量的测定。

英文摘要:

      Objective To establish a method for the determination of cyanide content in liquor by headspace gas chromatography-mass spectrometry (GC-MS). Methods The headspace equilibrium temperature, time, pH value and the amount of chloramine T were optimized, and the samples were detected by GC-MS with headspace sampler. The method was applied to detect 4 kinds of liquor including rice-flavor, fen-flavor, soybean-flavor and luzhou flavor that adding cyanide standard solution. Results Cyanide content in liquor had good linear relationships in the range of 0.0010.2mg/L, and the correlation coefficient (r2) was 0.9996. The limit of the detection was 0.01 mg/L (S/N≥3) and the limit of quantification was 0.03 mg/L (S/N≥10). The recoveries were 71.6%116.2%, with the relative standard deviations of 1.3% (n=6). Conclusion This method is simple in operation and high in accuracy. Compared with the gas chromatography method in the national standard, this method obviously shortens the detection period and improves the detection efficiency, which can be used for the determination of cyanide content in liquor.