环境卫生学杂志2024,Vol.14Issue(6) :508-513.DOI:10.13421/j.cnki.hjwsxzz.2024.06.008

两种湿消解法消解-原子荧光法测定尿中总砷

Two wet digestion methods for the determination of total arsenic in urine by digestion-atomic fluorescence spectrometry

杨志羡 包玉龙 李科 王慧 郭志伟
环境卫生学杂志2024,Vol.14Issue(6) :508-513.DOI:10.13421/j.cnki.hjwsxzz.2024.06.008

两种湿消解法消解-原子荧光法测定尿中总砷

Two wet digestion methods for the determination of total arsenic in urine by digestion-atomic fluorescence spectrometry

杨志羡 1包玉龙 1李科 1王慧 1郭志伟1
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作者信息

  • 1. 内蒙古自治区疾病预防控制中心地方病实验室,呼和浩特 010080
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摘要

目的 比较硝酸、硫酸、高氯酸混酸与过硫酸铵两种消解法-原子荧光测定尿中总砷的方法.方法 前处理分别用硝酸、高氯酸、硫酸混酸在 310℃下对尿样消解 1h后加硫脲-抗坏血酸还原样品和用饱和过硫酸铵溶液在 310℃下对尿样消解 1h后加入硫脲-抗坏血酸还原,进入原子荧光仪检测.结果 在 1.00~20.00 μg/L砷含量范围内,标准曲线回归方程:y=106.587x-11.979,相关系数优于 0.999 0,混酸消解法的精密度 2.06%~3.03%,平均加标回收率 101.2%~104.3%,检出限0.012 μg/L;饱和过硫酸铵消解法的精密度 3.31%~4.05%,平均加标回收率 97.9%~101.6%,检出限 0.006 μg/L.结论 两种方法的准确度、精密度均符合卫生标准《尿中砷的测定 氢化物发生原子荧光法》(WS/T 474-2015)的要求,适于大批量尿中总砷含量的检测.

Abstract

Objective To compare the two digestion methods of ammonium persulfate and the mixed acid system of nitric acid,sulfuric acid,and perchloric acid in determining total arsenic in urine by digestion-atomic fluorescence spectrometry.Methods Urine samples were digested by the mixed acid system of nitric acid,sulfuric acid,and perchloric acid and saturating ammonium persulfate at 310℃for 1 hour,then thiourea-ascorbic acid was added to reduce the sample,and the samples were placed in the atomic fluorescence spectrometry analyzer for determination.Results Within the range of 1.00-20.00 μg/L for the content of arsenic,the standard curve regression equation was y=106.587x-11.979,with a correlation coefficient of>0.999 0.The digestion method of the mixed acid sys-tem had a precision of 2.06%-3.03%,an average spike recovery of 101.2%-104.3%,and a detection limit of 0.012 μg/L.The saturating ammonium persulfate digestion method had a precision of 3.31%-4.05%,an average spike recovery of 97.9%-101.6%,and a detection limit of 0.006 μg/L.Conclusion The accuracy and precision of both methods meet the requirements in Determination of arsenic in urine by hydride generation atomic fluorescence spectrometry(WS/T 474-2015),and the two methods are suitable for large-scale determination of total arsenic content in urine.

关键词

湿消化/过硫酸铵/混酸/原子荧光/总砷

Key words

wet digestion/ammonium persulfate/mixed acid/atomic fluorescence spectrometry/total arsenic

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基金项目

中央引导地方科技发展资金项目(2021ZY0047)

西部青年学者项目(人字[2022]4号)

内蒙古自治区科技计划(2021GG0383)

内蒙古自治区卫生健康科技计划(202201161)

出版年

2024
环境卫生学杂志
中国疾病预防控制中心

环境卫生学杂志

CSTPCD
影响因子:0.735
ISSN:2095-1906
参考文献量10
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