吹扫捕集-气相色谱-质谱联用法测定白酒中氰化物  

Analysis of cyanide in liquor by purge and trap-gas chromatography-mass spectrometry

作　　者：张学[1] 朱建民[1] 彭立核[1] 谢爱萍[1] 朱福源[1] 

机构地区：[1]嘉善县疾病预防控制中心,浙江嘉善314100

出　　处：《中国食品卫生杂志》2016年第3期344-347,共4页Chinese Journal of Food Hygiene

摘　　要：目的建立一种应用吹扫捕集-气相色谱-质谱联用法测定白酒中氰化物的方法。方法白酒加入氢氧化钠调节pH值（使pH〉12）,在碱性条件下水浴蒸干白酒样品,再加入氯胺T和磷酸,以吹扫捕集-气相色谱-质谱联用法进行测定。结果本方法氰化物线性范围在10~200μg/L内,线性良好,线性方程为y=42563x＋24231,相关系数（r）为0.999 2。样品加标量为50、100、150μg/L时,回收率范围在75.8%~92.8%之间,相对标准偏差（RSD）范围为3.1%~7.8%;白酒中氰化物的定量限（LOQ）为50μg/L、检出限（LOD）为15μg/L。结论本文建立的白酒中微量氰化物测定方法操作简便、灵敏度高、结果可靠,适用于实验室对白酒中氰化物的定量检测。Objective To establish a method of purge and trap-gas chromatography-mass spectrometry method for the determination of cyanide in liquor.Methods Sodium hydroxide was added to the sample to adjust the p H to above 12,then the sample was water bathed to dry,and detected by purge and trap-gas chromatography-mass spectrometry after adding chloramine T and phosphoric acid.Results Cyanide was in the range of 10-200 μg/L with good linearity,the linear equation was y=42563 x ＋ 24231 with r = 0.999 2.The spiked samples were 50,100 and 150 μg/L,and the recovery rate was 75.8%-92.8% with RSD of 3.1%-7.8%.The detection limit was 10 μg/L.Conclusion The method is simple,accurate,and suitable for the determination of cyanide in wine.

关 键 词：吹扫捕集 白酒 氰化物 气相色谱-质谱联用法 食品污染物 

分 类 号：R155.59[医药卫生—营养与食品卫生学]