顶空气相色谱法测定白酒中氰化物含量

目的建立顶空气相色谱法测定白酒中氰化物含量检测的方法,探究GB5009.36-2016第二法在白酒、白兰地、威士忌、朗姆酒等酒样中应用的区别。方法将酒样进碱解前处理后,以顶空进样器注入气相色谱仪进行分离,电子捕获检测器进行检测。以加标回收率为指标,对方法及前处理进行评价。结果国标第一法与第二法结果有较大的差别,碱解前处理的气相色谱法与国标第一法结果相近。用GB 5009.36-2016第二法测定白酒、白兰地、威士忌、朗姆酒等中的氰化物含量时,均无法得到较好的加标回收率;用GB5009.36-2016第二法检测伏特加、以食用酒精为酒基的露酒中的氰化物含量时可以得到较好的回收率。顶空气相色谱法测定白酒中氰化物含量时,线性相关系数r为0.9999,相对标准偏差(relative standard deviation,RSD)为8.0%,回收率为78.0%～1112.5%。结论顶空气相色谱法测定白酒中氰化物含量时能够得到与国标第一法相近的结果,该方法操简单、灵敏度高,结果准确度高,适合白酒中氰化物含量的测定。

Determination of cyanide in liquor by headspace gas chromatography

Objective To establish a method for the determination of cyanide content in liquor by headspace gas chromatography, and to explore the difference between the application of GB 5009.36-2016 second method in liquors such as liquor, brandy, whiskey and rum. Methods After the wine sample was subjected to alkaline hydrolysis treatment, it was separated into a gas chromatograph by a headspace sampler, and an electron capture detector was used for detection.The method and pretreatment were evaluated by the spiked recovery rates. Results The results of the first method of the national standard and the second method were quite different. The gas chromatography with alkaline hydrolysis treatmentwas similar to the first method of the national standard.When the cyanide contents in white wine, brandy, whiskey, rum, etc. were determined by the second method of GB 5009.36-2016, no good spike recovery rate could be obtained. A better recovery rate could be obtained by detecting the cyanide content of vodka and the alcohol-based wine bythe second method of GB 5009.36-2016.When the cyanide contents in liquor were determined by headspace gas chromatography, the linear correlation coefficient r was 0.9999, the relative standard deviation (RSD) was 8.0%, and the recoveries were 78.0%-112.5%. Conclusion When the headspace gas chromatography method is used to determine the cyanide content in liquor, the results similar to the first method of the national standard can be obtained. The method is simple in operation, high in sensitivity and high in accuracy, which is suitable for the determination of cyanide content in liquor.