CAJ | 학술논문

目的对尿中碘的砷铈催化分光光度测定方法(WS/T 107-2006)的修订方法进行验证.方法参照《生物材料中化学物质的测定方法》,对方法中不碘浓度与吸光度的线性关系、最低检出浓度、样品测定精密度、准确度进行验证.结果不同范围(0～300μg/L、300 ～ 1200 μg/L)碘质量浓度(C)与相应吸光度(A)的相关系数(r)分别为-0.9998～-1.0000(n=6)、-0.9998～-1.0000(n=6)；最低检出碘浓度为1.3 μg/L:精密度:对含碘为71.3～244.9 μg/L 3个尿样和388.5 ～ 1018.0μg/L的3个尿样各重复测定6次,相对标准差(RSD)分别为1.5％(1.1/71.3)～2.5％(6.2/244.9)、0.6％(2.4/388.5)～1.7％(17.3/1018.0).准确度:测定碘73.0和206.0 μg/L 2种尿碘标准物质(n=6),相对误差(RD)分别为1.8％(1.3/73.0)、0.4％ (0.8/206.0)；测定碘556.0 μg/L和883.0 μg/L 2种高尿碘标准物质(n=6),RD分别为0.2％ (1.0/556.0)、-1.6％(-13.7/883.0),测定结果均在给定值的不确定度范围内.对含碘64.6 ～ 144.9 μg/L的3个尿样和346.8 ～ 574.4 μg/L的3个尿样加碘标回收实验,回收率范围为93.2％(186.3/200.0)～103.4％(51.7/50.0),总平均为98.8％.结论修订后的尿碘测定方法大幅减少了废液含砷量,并可无需稀释直接取高碘尿样进行消化测定,方法标准曲线线性关系好、精密度好、准确度高,符合生物样品分析的要求.
목적 대뇨중전적신시최화분광광도측정방법(WS/T 107-2006)적수정방법진행험증.방법 삼조《생물재료중화학물질적측정방법》,대방법중불전농도여흡광도적선성관계、최저검출농도、양품측정정밀도、준학도진행험증.결과 불동범위(0～300μg/L、300 ～ 1200 μg/L)전질량농도(C)여상응흡광도(A)적상관계수(r)분별위-0.9998～-1.0000(n=6)、-0.9998～-1.0000(n=6)；최저검출전농도위1.3 μg/L:정밀도:대함전위71.3～244.9 μg/L 3개뇨양화388.5 ～ 1018.0μg/L적3개뇨양각중복측정6차,상대표준차(RSD)분별위1.5％(1.1/71.3)～2.5％(6.2/244.9)、0.6％(2.4/388.5)～1.7％(17.3/1018.0).준학도:측정전73.0화206.0 μg/L 2충뇨전표준물질(n=6),상대오차(RD)분별위1.8％(1.3/73.0)、0.4％ (0.8/206.0)；측정전556.0 μg/L화883.0 μg/L 2충고뇨전표준물질(n=6),RD분별위0.2％ (1.0/556.0)、-1.6％(-13.7/883.0),측정결과균재급정치적불학정도범위내.대함전64.6 ～ 144.9 μg/L적3개뇨양화346.8 ～ 574.4 μg/L적3개뇨양가전표회수실험,회수솔범위위93.2％(186.3/200.0)～103.4％(51.7/50.0),총평균위98.8％.결론 수정후적뇨전측정방법대폭감소료폐액함신량,병가무수희석직접취고전뇨양진행소화측정,방법표준곡선선성관계호、정밀도호、준학도고,부합생물양품분석적요구.
Objective To verify a new revised method with low usage amount of arsenic trioxide for determining urinary iodine by As(Ⅲ)-Ce4+ catalytic spectrophotometry using ammonium persulfate digestion.Methods The standard curve linearity,sample detection limit,precision and accuracy of determining urinary iodine of this modified method were verified according to "Determination Methods of Chemicals in Biological Materials".Results The linear correlative coefficients of the 0-300 μg/L range and 300-1200 μg/L range calibration curve were-0.9998--1.0000(n =6) and-0.9998--1.0000,respectively.The detection limit for iodine was 1.3 μg/L.The relative standard deviations were 1.5％ (1.1/71.3)-2.5％ (6.2/244.9) when measuring 3 urine samples with iodine concentration of 71.3-244.9 μg/L,and 0.6％(2.4/388.5)-1.7％(17.3/1018.0) when measuring 3 urine samples with iodine concentration of 388.5-1018.0 μg/L,respectively(n =6).The test results of the four urinary iodine national standard materials with iodine concentration of 73.0,206.0,556.0 and 883.0 μg,/L were all within the given value range and the average value relative deviation was 1.8％ (1.3/73.0),0.4％ (0.8/206.0),0.2％ (1.0/556.0) and-1.6％(-13.7/883.0),respectively (n =6).The average recovery was 98.8％ with a range of 93.2％ (186.3/200.0)-103.4％(51.7/50.0) when measuring 3 urine samples with iodine concentration of 64.6-144.9 μg/L and 3 urine samples with iodine concentration of 346.8-574.4 μg/L,respectively.Conclusions This new modified method greatly reduces the amount of waste containing arsenic,and can directly take urine samples with high iodine concentration to digest and determine without dilution.It is performed with good standard linear curve,better precision and high accuracy,and in line with the analysis of biological samples requirements.