衍生化法测定尿中碘化物

Measurement of Iodide in Urine by Derivatization Capillary Gas Chromatography

目的建立尿中碘化物的气相色谱测定方法。方法采用重铬酸钾、硫酸、丁酮与碘酸钾反应,用苯作萃取剂,HP-5毛细管柱分离,ECD检测器检测,峰面积定量。结果本法检出限为0.025μg/ml,I-在0～1.0μg/ml浓度范围内呈良好线性关系,平均回收率为82.7%～93.2%,相对标准偏差(RSD)为3.0%,与砷铈法比较,差异无统计学意义(P>0.05)。尿中氟化物、氯化物不干扰碘化物的测定。结论该法操作简便、灵敏、准确可靠,用于实际尿样的测定,具有较高应用价值。

Objective To build a derivatization capillary gas chromatography for determining iodide in urine. Methods Adopting reaction of pedantic dichromic potassium, sulfuric acid, butanone with iedic acid potassium, iodine was detected in urine with benzene as extraction agent, HP- 5 capillary column separation, ECD detection, and peak area quantification. Results The detection limit was 0. 025μg/ml, the linear relation of I^- was excellent within the range of 0-1.0 μg/ml, and the mean recovery rate was between 82.7% and 93.2 %, with relative standard deviation （RSD） of 3.0%. As compared with the arsenic cerium method, no significant difference was found between the two methods （P 〉0.05）. The urine fluoride and chloride did not interfere with the determination of iodide. Conclusions The method has the advantages of easy operation, high sensitivity, good accuracy and reliability, and high clinical applicative value in determination of urine sample.