离子色谱-脉冲安培法测定白酒中氰化物
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(1.国家食品安全风险评估中心,北京 100022;2.中粮营养健康研究院有限公司, 北京 102209;3.中粮生物科技(北京)

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王紫菲 女 助理研究员 研究方向为食品安全理化检测方法和标准 E-mail:wangzifei@cfsa.net.cn 郭杰 女 研发专员 研究方向为食品理化相关检测分析 E-mail:guojie6@cofco.com

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“十三五”国家重点研发计划专项项目(2018YFC1604101)


Development of an analytical method to detect cyanide in Chinese liquor by ion chromatography with pulsed amperometric detection
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(1.China National Center for Food Safety Risk Assessment, Beijing 100022,China;2.Nutrition & Health Research Institute, China Oil & Foodstuffs Corporation, Beijing 102209,China;3.China Oil & Foodstuffs Corporation Biotech (Beijing) Co., Ltd., Beijing 102209,China)

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    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5~200 μg/L浓度范围内线性关系良好,相关系数R2为0.999 9。该方法对白酒类基质检出限为3.5 μg/L,定量限为9.5 μg/L。对不同类型白酒样品,在10、30和50 μg/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。

    Abstract:

    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.

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王紫菲,苗宏健,骆鹏杰,孙铁虎,郑晓卫,郭杰.离子色谱-脉冲安培法测定白酒中氰化物[J].中国食品卫生杂志,2020,32(3):257-261.

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  • 收稿日期:2020-05-11
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  • 在线发布日期: 2020-07-03
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