摘要
目的探索自控消解仪新技术在尿中砷检测前处理的应用,实现对样品快速、便捷、准确的检测效果。方法采用湿法消解法,利用氢化物发生-原子荧光光度法(HG-AFS),建立一套先进的样品前处理消解方法(简称新前处理技术)。取1.0 ml尿样,置于10.0 ml具塞刻度消化管中,依次加入0.20 ml硫酸、0.30 ml硝酸、0.50 ml过氧化氢摇匀,置于160℃AED-IV型自控消解仪中,消解0.5 h后升温至200℃,消解1 h后,再持续升温至260℃,消解至液体为无色(或淡黄色)透明、液面平静、回流均匀。消解结束,用原子荧光光度计测定。对新前处理技术与现行标准(WS/T 474-2015)方法进行比较,计算标准曲线及线性范围,样品测定的检测限、精密度、准确度。结果新前处理技术每次可消化样品60份,优于现行标准方法(20份),且降低了试剂的使用量,两种方法的测定结果比较差异无统计学意义(P>0.05)。在0~100μg/L线性范围内时,采用新前处理技术,标准曲线相关系数(r)>0.9993,方法检测限为0.066μg/L,相对标准偏差(RSD)<5%。结论新前处理技术快速高效、环保经济、自动化程度高,实验结果误差在可控范围,能用于不同浓度尿中砷含量的消解,具有很高的适用性。
Objective To explore the application of new pretreatment technology of automatic electrothermal digestion instrument in the detection of arsenic in urine samples,in order to achieve rapid,convenient and accurate detection results.Methods Using wet digestion,an advanced sample preparation and digestion method(referred to as new pretreatment technology)was established by hydride generation-atomic fluorescence spectrometry(HG-AFS).Wet digestion:took 1.0 ml urine samples and put them into 10.0 ml corked scale digestive tubes,and added 0.20 ml sulfuric acid,0.30 ml nitric acid and 0.50 ml hydrogen peroxide into the tubes successively.Shook solution and put them at AED-IV automatic electrothermal digestion instrument with 160℃for half an hour,then heated up to 200℃for 1 hour.It needed to be continually heated up to 260℃and dissolved the solution until colorless transparent or light yellow.When the liquid level calm,and uniform reflux appeared,which meant the digestion finished,and then measured by atomic fluorescence photometer.At the same time,the new pretreatment technology was compared with the current standard(WS/T 474-2015)method,and the standard curve and linear range were calculated,as well as the detection line,precision and accuracy of the sample measurement.Results The new pretreatment technology could digest 60 samples per sample,which was superior to the current standard methods(20 samples)and reduced the amount of reagent used.There was no statistically significant difference between the two methods(P>0.05).In the linear range of 0-100μg/L,the correlation coefficient(r)>0.9993,the detection limit of the method was 0.066μg/L,and the relative standard deviation(RSD)<5%.Conclusions The new pretreatment technology is fast,efficient,environmentally friendly,economical,highly automated.The experimental result error is in a controllable range.It can be used for digestion of arsenic content in urine of different concentrations and has high applicability.
作者
潘月华
潘炯波
郭华
张念恒
裴莉
黄伊彦文
Pan Yuehua;Pan Jiongbo;Guo Hua;Zhang Nianheng;Pei Li;Huang Yiyanwen(Department of Quality Control,Experimental Center,Guizhou Center for Disease Control and Prevention,Guiyang 550004,China;Chemistry Room,Sandu County Ethnic Middle School,Sandu 558100,China;Advanced Food Safety,Queen's University Belfast,Belfast BT71NN,England)
出处
《中华地方病学杂志》
CAS
CSCD
北大核心
2019年第11期936-940,共5页
Chinese Journal of Endemiology
关键词
尿
砷
AED-IV型自控消解仪
Urine
Arsenic
AED-IV automatic electrothermal digestion instrument
作者简介
通信作者:黄伊彦文,Email:hy011027@qq.com,电话:18585059133。
