尿中碘的过硫酸铵消化-低砷量砷铈催化分光光度测定方法  

Revised method with low usage amount of arsenic trioxide for testing urinary iodine by As （ HI ）-Ce4＋ catalytic spectrophotometry using ammonium persulfate digestion

作　　者：张亚平[1] 阎玉芹[2] 刘列钧[3] 孙毅娜[2] 李卫东[4] 华基礼[5] 黄嫣红[1] 李秀维[3] 赵立胜[4] 

机构地区：[1]福建省厦门市疾病预防控制中心检验科,361021 [2]天津医科大学内分泌研究所 [3]中国疾病预防控制中心传染病预防控制所 [4]安徽省疾病预防控制中心 [5]陕西省地方病防治研究所

出　　处：《中华地方病学杂志》2013年第1期95-100,共6页Chinese Journal of Endemiology

基　　金：卫生部卫生标准制修项目（20111801）

摘　　要：目的介绍修订后的尿碘测定标准方法，即尿中碘的过硫酸铵消化一低砷量砷铈催化分光光度测定方法。方法修订后的新方法包括：改进的0．0～300．0μg／L范围尿碘测定步骤、新增加的300．0。1200．0μg／L范围尿碘测定步骤，每份尿碘检测所用的亚砷酸试剂量仅为现行标准法的1／4。对修订后的新方法进行评价，计算标准曲线线性关系及线性范围、样品测定检测限、精密度、准确度。结果尿碘含量为O．O～300．0μg／L、300．0—1200．0μg／L的标准曲线按碘质量浓度（C）与测定吸光度（A）的定量关系为（C=a＋b×lga），线性相关系数范围分别为一0．9995—-1．0000、-0．9994—-1．0000；尿碘检出限为2．0Ixg／L（取样量为0．25mm）；精密度：对尿碘35．6～265．5Ixg／L的12个尿样各重复测定6次，相对标准偏差（RSD）范围为0．9％（0．6／70-3）～3．3％（1．2／35．6），平均为1．8％；对尿碘330．0～1112．0μg／L的12个尿样各重复测定6次，RSD范围为0．4％（2．0／517．3）一2．2％（7．2／330．1），平均为1．2％。准确度：对尿碘33．7～203．0μg／L的15个尿样加碘标回收率范围为93．8％（93．8／100）～103．9％（103．9／100），平均为99.4％；对含碘330．0—783．0阻g／L的15个尿样加碘标回收率范围为91．2％（501．8／550）-102．9％（411．7／400），平均为98．2％；分别在不同反应温度下测定尿碘73．0、88．0、175．0、206．0、212．0μg／L的5种尿碘标准物，相对误差范围为-2．8％（-5．9／212）～3．9％（6．9／175）；测定尿碘556．0μg／L和883．0μg／L的2种高尿碘标准物，相对误差范围为-0．7％（-7．0／883）-1．5％（8．1／556），测定结果均在给定值的不确定度范围内。结论修订后的新方法比原标准方法大幅减少了废液含砷量，减少了环境污染并节省了试剂。可直接取高碘尿Objective To introduce a newly revised method for determination of urinary iodine with low usage amount of arsenic trioxide and by As（ m ）-Ce4＋ catalytic spectrophotometry using ammonium persulfate digestion. Methods The newly revised method include ：improved detection steps of 0.0 - 300.0 txg/L range urinary iodine, and increased detection steps of 300.0 - 1200.0 I^g/L range urinary iodine, usage amount of arsenious acid solution was only a quarter of usage amount of the current standard method. The new modification for the national standard method was introduced and the method was evaluated on standard curve linearity and linear range, sample detection limit, precision and accuracy. Results The linear correlation coefficients of the 0.0 - 300 μg/L range and 300.0 - 1200.0 μg/L range calibration curve[C = a ＋ b lgA, C：iodine concentration, A ： measuring absorbanee] were - 0.9995 - - 1.0000, - 0.9994 - - 1.0000, respectively. The detection limit for iodine was 2.0 μg/L（0.25 ml of urine was tested）. The relative standard deviations were 0.9% （0.6/70.3） - 3.3% （1.2/35.6） when measuring 12 urine samples with iodine concentration of 35.6 - 265.5 Ixg/L,and 0.4%（2.0/517.3） - 2.2%（7.2/330.1） when measuring 12 urine samples with iodine concentration of 330.0 - 1112.0 Ixg/L. The average recovery was 99.4% with a range of 93.8%（93.8/100） - 103.9%（103.9/100） when measuring 15 urine samples with iodine concentration of 33.7 - 203.0 Ixg/L, and was 98.2% with a range of 91.2%（501.8/550） - 102.9%（411.7/400） when measuring 15 urine samples with iodine concentration of 330.0 - 783.0 Ixg./L. At different test temperature, the test results of five urinary iodine national standard materials with iodine concentration of 73.0, 88.0, 175.0, 206.0, 212.0 IJ.g/L were all within the given value range and the relative deviation range was - 2.8%（ - 5.9/212） - 3.9%（6.9/175）, and the test results of two urinary iodine national standard materials with iodine concentration of 556.0 a

关 键 词：碘 尿 标准修订 分光光度法 砷 

分 类 号：R446.1[医药卫生—诊断学]