摘要
目的建立离子色谱-脉冲安培法检测白酒中氰化物含量的方法。方法白酒样品稀释10倍后直接进样,以氢氧化钾溶液(12 mmol/L)进行等梯度淋洗,采用银工作电极,以Ag/AgCl复合参比电极模式,脉冲安培三点位波形方式进行检测。结果该方法在5~200μg/L浓度范围内线性关系良好,相关系数R^2为0.999 9。该方法对白酒类基质检出限为3.5μg/L,定量限为9.5μg/L。对不同类型白酒样品,在10、30和50μg/L三个加标浓度水平下回收率在91.7%~102.0%之间。日内相对标准偏差(RSD)在2.2%~4.8%之间,日间RSD在1.5%~1.9%之间。本方法与GB 5009.36-2016《食品安全国家标准食品氯化物的测定》中的气相色谱法进行比较,结果差异无统计学意义(P>0.05)。结论该方法操作步骤简单快速,结果准确可靠,适用于实际白酒样品中氰化物的检测。
Objective This study aimed to develop an ion chromatography-pulse amperometry(IC-PAD) technique for the identification and quantification of cyanide in Chinese liquor. Methods The real samples from local markets were diluted to 1∶10 with ultrapure water before being injected to IC-PAD. Potassium hydroxide(12 mmol/L)was introduced for gradient elution. Silver electrode was utilized with Ag/AgCl composite reference electrode mode. Three potential wave forms were also involved in the study. Results This method showed good linear responses ranging from 5 to 200 μg/L with satisfactory linear correlation coefficient of 0.999 9. The limit of detection(LOD) was 3.5 μg/L, and the limit of quantitation(LOQ) was 9.5 μg/L in Chinese liquor samples. For different types of Chinese liquor, the recoveries of cyanide in fortified samples(10, 30, 50 μg/L) were from 91.7% to 102.0%. The intra-day relative standard deviation(RSD) was from 2.2% to 4.8%, and the inter-day RSD ranged from 1.5% to 1.9%. The comparison between this proposed method and the GB 5009.36-2016 method showed no statistical difference(P>0.05). Conclusion This technique was performer-friendly and exhibited high reliability and accuracy, which was suitable for the detection of cyanide in real samples.
作者
王紫菲
苗宏健
骆鹏杰
孙铁虎
郑晓卫
郭杰
WANG Zifei;MIAO Hongjian;LUO Pengjie;SUN Tiehu;ZHENG Xiaowei;GUO Jie(China National Center for Food Safety Risk Assessment,Beijing 100022,China;Nutrition&Health Research Institute,China Oil&Foodstuffs Corporation,Beijing 102209,China;China Oil&Foodstuffs Corporation Biotech(Beijing)Co.,Ltd.,Beijing 102209,China)
出处
《中国食品卫生杂志》
CSCD
北大核心
2020年第3期257-261,共5页
Chinese Journal of Food Hygiene
基金
“十三五”国家重点研发计划专项项目(2018YFC1604101)。
关键词
白酒
离子色谱
脉冲安培
氰化物
Chinese liquor
ion chromatography
pulsed amperometric
cyanide
