CAJ | 학술논문

目的验证修订后的砷铈催化分光光度方法测定尿碘的可行性及应用价值.方法收集成人1次性尿样备用,制备0～300μg/L和300～ 1200 μg/L的碘标准曲线,应用修订后的砷铈催化分光光度方法测定尿碘.对该检测方法的线性关系及范围、最低检测限、精密度和准确度进行验证,评价验证结果.结果当标准曲线线性范围在0 ～ 300 μg/L时,最低检出限为1.8 μg/L,相关系数为-0.9995～-0.9997;测定尿碘浓度为40～ 80、100～ 149、200～280 μg/L尿样时,相对标准差分别为1.5％、0.8％、0.5％；测定尿碘浓度为40 ～ 80、100～149、150～180 μg/L尿样时,加标回收率分别为97.8％、99.8％、96.6％；国家尿碘标准物给定值(标准值±不确定度)为(73.0±9.0)、(206±10) μg/L时,测定值为(75.5±0.9)、(207.5±1.9)μg/L,相对偏差分别为3.4％和0.7％,测定结果在不确定度范围内.当标准曲线线性范围为300～1200μg/L时,最低检出限为305.2μg/L,相关系数为-0.9996～-0.9999;测定尿碘浓度为300～ 400、500～600、1000～ 1200μg/L尿样时,相对标准差分别为0.6％、1.0％、0.7％；测定尿碘浓度为300～ 499、500～ 599、600 ～700μg/L尿样时,加标回收率分别为99.7％、99.2％、100.4％;国家尿碘标准物给定值(标准值±不确定度)为(556.0±17.0)、(883.0±28.0)μg/L时,测定值为(558.3±3.5)、(884.8±4.7)μg/L,相对偏差分别为0.4％和0.2％,测定结果在不确定度范围内.结论经验证,新修订的砷铈催化分光光度方法不仅能扩展尿碘检测范围,保证尿碘测定的精密度和准确度,由于能减少实验中砷的使用量,减轻对环境污染,适合推广应用.
목적 험증수정후적신시최화분광광도방법측정뇨전적가행성급응용개치.방법 수집성인1차성뇨양비용,제비0～300μg/L화300～ 1200 μg/L적전표준곡선,응용수정후적신시최화분광광도방법측정뇨전.대해검측방법적선성관계급범위、최저검측한、정밀도화준학도진행험증,평개험증결과.결과 당표준곡선선성범위재0 ～ 300 μg/L시,최저검출한위1.8 μg/L,상관계수위-0.9995～-0.9997;측정뇨전농도위40～ 80、100～ 149、200～280 μg/L뇨양시,상대표준차분별위1.5％、0.8％、0.5％；측정뇨전농도위40 ～ 80、100～149、150～180 μg/L뇨양시,가표회수솔분별위97.8％、99.8％、96.6％；국가뇨전표준물급정치(표준치±불학정도)위(73.0±9.0)、(206±10) μg/L시,측정치위(75.5±0.9)、(207.5±1.9)μg/L,상대편차분별위3.4％화0.7％,측정결과재불학정도범위내.당표준곡선선성범위위300～1200μg/L시,최저검출한위305.2μg/L,상관계수위-0.9996～-0.9999;측정뇨전농도위300～ 400、500～600、1000～ 1200μg/L뇨양시,상대표준차분별위0.6％、1.0％、0.7％；측정뇨전농도위300～ 499、500～ 599、600 ～700μg/L뇨양시,가표회수솔분별위99.7％、99.2％、100.4％;국가뇨전표준물급정치(표준치±불학정도)위(556.0±17.0)、(883.0±28.0)μg/L시,측정치위(558.3±3.5)、(884.8±4.7)μg/L,상대편차분별위0.4％화0.2％,측정결과재불학정도범위내.결론 경험증,신수정적신시최화분광광도방법불부능확전뇨전검측범위,보증뇨전측정적정밀도화준학도,유우능감소실험중신적사용량,감경대배경오염,괄합추엄응용.
Objective To verify the feasibility and application value of an improved method for determination of urinary iodine by As3+-Ce4+ catalytic spectrophotometry.Methods Adults urine samples were collected,iodine calibration curves of 0-300 μg/L and 300-1200 μg/L were prepared,and urinary iodine was determined by the improved As3+-Ce4+ catalytic spectrophotometric method.Lyophilized human urinary iodine ingredient standards were used to validate linearity and range,limit of detection,precision and accuracy of this improved detection method.Results The linear range of the calibration curve was 0-300 μg/L,the detection limit was 1.8 μg/L,and the range of correlation coefficient was-0.9995--0.9997.When measuring urinary iodine at 40-80,100-149,200-280 μg/L,the relative standard deviations were 1.5％,0.8％ and 0.5％.When measuring urinary iodine at 40-80,100-149,150-180 μg/L,the average recoveries were 97.8％,99.8％ and 96.6％.Two given values of urinary iodine of national standard samples were (73.0± 9.0) and (206.0± 10.0)μg/L,and the results determined by this method were (75.5 + 0.9) and (207.5 ± 1.9)μg/L,and the relative deviation was 3.4％ and 0.7％,respectively,the results determined were all within the given value range.The linear range of the calibration curve was 300-1200 μg/L,the detection limit was 305.2 μg/L,the range of the correlation coefficient was-0.9996--0.9999.When measuring urinary iodine at 300-400,500-600 and 1000-1200μg/L,the relative standard deviations were 0.6％,1.0％ and 0.7％.When measuring urinary iodine at 300-499,500-599 and 600-700 μg/L,the average recoveries were 99.7％,99.2％ and 100.4％.Two given values of urinary iodine of national standard samples were (558.3 ± 3.5) and (884.8 ± 4.7)μg/L,the results determined by this method were (556.0 + 17.0) and (883.0 ± 28.0)μg/L,and the relative deviation was 0.4％ and 0.2％,respectively,the results were all within the given value range.Conclusions This method extends the detection range of iodine concentration,and improves precision and accuracy.This method greatly reduces the amount of arsenic used therefore reduces environmental pollution,which is suitable for promotion.