摘要
目的建立全自动消解氢化物发生原子荧光光谱法测定婴幼儿米粉中砷的分析方法。方法样品经全自动消解仪消解,优化后的升温程序以10℃/min升至90℃,保持30min,再以5℃/min升至130℃,保持60min,以5℃/min升至150℃,保持80min,再以15℃/min升至205℃,保持60min,最后再以10℃/min升至220℃,保持50min,加入2ml硫脲-抗坏血酸,然后消解仪由定容程序加超纯水自动定容至25ml,经参数优化后的氢化物发生原子荧光光谱仪测定,外标法定量。结果方法线性范围为0ng/ml^10ng/ml,相关系数为0.9995,检出限为0.02mg/kg,加标回收率为93.8%~103.0%,相对标准偏差为2.1%~3.9%,测定结果与质控大米粉参考值相符。结论本法操作简便、灵敏、准确,能够满足婴幼儿米粉的测定要求,可用于米粉样品中总砷测定。
Objective To establish a method for the determination of total arsenic in infant flour by using automatical digestion-hydride generation atomic fluorescence spectrometry.Methods The samples were digested by using automatic digestion instrument.The optimized temperature rise procedure was as follows:Raised to 90℃at the rate of 10℃/min,keeping for 30 min,then raised to 130℃at the rate of 5℃/min for 60 min,raised to 150℃at the rate of 5℃/min,keeping for 80 min,then raised to 205℃at the rate of 15℃/min,keeping for 60 min,and finally raised to 220℃at the rate of 10℃/min,keeping for 50 min,then added 2 ml thiourea-ascorbic acid and ultra-pure water to 25 ml.Arsenic in digested solution was determined by atomic fluorescence spectrometry.The quantification was based on external standard method.Results The method linearity was within 0 ng/ml-10 ng/ml,with the correlation coefficient of 0.999 5.The recoveries were within 93.8%-103.0%,with relative standard deviation in the range of 2.1%-3.9%.The limit of detection was 0.02 mg/kg.The measurement results of the quality control rice flour were within the given values.Conclusion The proposed method is simple,sensitive and accurate,which meets the measurement requirements of infant rice and can be used for the determination of total arsenic in infant rice flour samples.
作者
李文鹏
贾勇
王丽群
蒋尧
文金
LI Wen-peng;JIA Yong;WANG Li-qun;JIANG Yao;WEN Jin(Ziyang Center for Disease Control and Prevention,Ziyang,Sichuan 641300,China)
出处
《中国卫生检验杂志》
CAS
2019年第20期2475-2477,2487,共4页
Chinese Journal of Health Laboratory Technology
关键词
全自动消解
原子荧光光谱法
婴幼儿米粉
砷
Full-automatic digestion
Atomic fluorescence spectrometry
Infant rice flour
Arsenic
作者简介
李文鹏(1985-),男,硕士,工程师,主要从事化学分析工作;通讯作者:贾勇,E-mail:349185203@qq.com。
