食品科学

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钨丝捕获-电热蒸发原子荧光光谱法直接测定饮料中痕量镉

王金玉,黄亚涛,毛雪飞,王 敏,焦必宁,张 英   

  1. 1.中国农业科学院农业质量标准与检测技术研究所,农业部农产品质量安全重点实验室,北京 100081;
    2.中国饮料工业协会,北京 100027;3.中国农业科学院柑桔研究所,重庆 400712
  • 出版日期:2013-12-25 发布日期:2014-01-03

direct sampling;tungsten coil trapping;electrothermal vaporization (ETV);atomic fluorescence spectrometry (AFS);beverages;ultra-trace cadmium

WANG Jin-yu,HUANG Ya-tao,MAO Xue-fei,WANG Min,JIAO Bi-ning,ZHANG Ying   

  1. 1. Key Laboratory of Agro-product Quality and Safety, Ministry of Agriculture, Institute of Quality Standard and Testing Technology for Agro-products, Chinese Academy of Agricultural Sciences, Beijing 100081, China;
    2. China Beverage Industry Association, Beijing 100027, China;
    3. Citrus Research Institute, Chinese Academy of Agricultural Sciences, Chongqing 400712, China
  • Online:2013-12-25 Published:2014-01-03

摘要:

利用钨丝特异性捕获镉(Cd)消除基体干扰,泡沫碳材质电热蒸发器串联原子荧光光谱仪,建立直接进样测定饮料痕量Cd的方法。仪器条件为:泡沫碳材质样品舟进样(10μL),采用灰化(矿泉水100W保持30s,其他饮料基质100W保持50s)与蒸发(70W保持30s)过程分离,Ar-H2(9:1)载气流速为600mL/min。结果表明:方法具有良好的线性,线性范围为0~5ng,相关系数r在0.998以上;10种饮料产品的加标回收率为92.2%~111.8%;方法检出限为0.04μg/L,相对标准偏差(RSD)在10%以内。本方法简单、灵敏、快速(包括样品前处理的分析时间不超过3min),适用于饮料产品痕量Cd的现场快速检测。

关键词: 直接进样, 钨丝捕获, 电热蒸发, 原子荧光光谱, 饮料, 痕量镉

Abstract:

A novel direct sampling method to determine cadmium in beverages by solid sampling electrothermal
vaporization atomic fluorescence spectrometry (SS-ETV-AFS) was established, where a tungsten coil as a Cd trap was used
to remove matrix interferences and foam graphite as an electrothermal vaporizer and a sample boat. In the present
study, 10 μL sample was loaded onto a sample boat, and then vaporized with 70 W for 30 s after being ashed
wi th 100 W for 30 s (natural spring water) or 50 s (beverages), using Ar/H2 (9:1) as the carrier gas with a flow
rate of 600 mL/min. Results showed that the calibration curve for Cd had good linearity (from 0 to 5 ng), and a correlation
coefficient (r) was more than 0.998; the recovery rates for Cd in 10 kinds of beverages were 92.2%-111.8%. The detection
limit was 0.04 μg/L, and the relative standard deviations (RSD) were less than 10%. This method is simple, sensitive,
fast (the whole analytical process including sample pretreatment can be completed within 3 min) and suitable for in-field
determination of ultra-trace amounts of Cd in beverages.

Key words: direct sampling, tungsten coil trapping, electrothermal vaporization (ETV), atomic fluorescence spectrometry (AFS), beverages, ultra-trace cadmium