CAJ | 학술논문

目的建立微量尿碘的低砷铈催化分光光度测定法,减少废液砷对环境的污染,批量测定微量尿碘.方法以过硫酸铵消化-砷铈催化分光光度法测定尿碘的原理为基础,96微孔板作为消化、催化反应容器,恒温烘箱作为消化加热工具,冰板降温,利用酶标仪测定吸光度值,建立微量尿碘低砷铈催化分光光度测定法(以下简称新方法).分析新方法性能(包括检出限实验、精密度实验、尿碘标准物测定、样品加标回收实验),并用新方法与我国尿碘定量检测的标准方法[《尿中碘的砷铈催化分光光度测定方法》(WS/T 107-2006),以下简称标准法]同时测定24份人尿样(高、中、低碘含量尿样各8份),将尿碘结果进行对比分析,验证新方法的准确度.结果新方法检测尿碘线性范围为0～300 μg/L;标准尿碘含量与测得吸光度值的对数之间相关系数(r)≥0.999;检出限为8.67 μg/L;高、中、低碘含量尿样检测值变异系数(CV)分别为2.15％、4.33％、3.48％;高、中、低碘含量标准物质检测值相对偏差(RD)分别为-0.16％、1.81％、-2.82％;低碘含量尿样加标回收率为97.51％,高碘含量尿样加标回收率为96.01％.新方法与标准法检测尿碘结果有统计学相关性(r=0.995,P＜0.05).结论新方法明显减少废液含砷量,降低环境污染,试剂用量节省,操作简便快捷,结果准确可靠,适合作为微量尿碘批量测试的补充方法推广.
목적 건립미량뇨전적저신시최화분광광도측정법,감소폐액신대배경적오염,비량측정미량뇨전.방법 이과류산안소화-신시최화분광광도법측정뇨전적원리위기출,96미공판작위소화、최화반응용기,항온홍상작위소화가열공구,빙판강온,이용매표의측정흡광도치,건립미량뇨전저신시최화분광광도측정법(이하간칭신방법).분석신방법성능(포괄검출한실험、정밀도실험、뇨전표준물측정、양품가표회수실험),병용신방법여아국뇨전정량검측적표준방법[《뇨중전적신시최화분광광도측정방법》(WS/T 107-2006),이하간칭표준법]동시측정24빈인뇨양(고、중、저전함량뇨양각8빈),장뇨전결과진행대비분석,험증신방법적준학도.결과 신방법검측뇨전선성범위위0～300 μg/L;표준뇨전함량여측득흡광도치적대수지간상관계수(r)≥0.999;검출한위8.67 μg/L;고、중、저전함량뇨양검측치변이계수(CV)분별위2.15％、4.33％、3.48％;고、중、저전함량표준물질검측치상대편차(RD)분별위-0.16％、1.81％、-2.82％;저전함량뇨양가표회수솔위97.51％,고전함량뇨양가표회수솔위96.01％.신방법여표준법검측뇨전결과유통계학상관성(r=0.995,P＜0.05).결론 신방법명현감소폐액함신량,강저배경오염,시제용량절성,조작간편쾌첩,결과준학가고,괄합작위미량뇨전비량측시적보충방법추엄.
Objective To introduce a new economical method which can be used for determination of urinary iodine of batch samples with low cost of arsenic trioxide,and decrease environmental pollution.Methods A catalytic spectrophotometry for measuring iodine content in a small volume of urine samples with low cost of arsenic and cerium was established based on the principle of ammonium persulfate digestion As3+-Ce4+ catalytic spectrophotometry.Ninety-six well polypropylene microplate was utilized as digestion and catalysis reaction vessel,conventional laboratory oven was used as a tool to digest and heat,ice plate was used to cool,and the absorbance was read with the Multimode Reader.The accuracy of the new method was evaluated with the current standard method (WS/T 107-2006) by simultaneous determination of urinary iodine of 24 urine samples.Results The linear range of this method was 0-300 μg/L,the linear correlative coefficient (r) was higher than 0.999,and the detection limit was 8.67 μg/L.The coefficient of variations was 2.15％,4.33％ and 3.48％ when measuring urine samples with high,medium and low iodine concentration,respectively.The test results of three national standard urinary iodine samples were all within the given value range and the relative deviation (RD) was-0.16％,1.81％ and-2.82％,respectively.The average recovery of the low concentration was 97.51％,and that of the high concentration was 96.01％.The two methods correlated well (r =0.995,P ＜ 0.01).Conclusions This method greatly reduces the arsenic waste,environmental pollution,consumables and labor.The new method is simple and efficient,accurate and reliable;it is suitable for application as a supplementary method for analyzing urinary iodine of a large number of samples.