流动注射-分光光度法联用测定药物制剂中维生素K_3的含量

Flow Injection Spectrophotometric Determination of Vitamine K_3 in Pharmaceuticals Preparation

把流动注射和分光光度联用建立了一种新的测定维生素K3的方法.把250μL维生素K3(Menadionesodiumbisulfite,MSB)水溶液注入到载流(水)中,试样带在流动的过程中与33%二甲胺水溶液汇流,在长100cm内径0.5mm的聚乙烯反应管中快速显色,生成一紫红色配合物,510nm为其最大吸收波长,本法检测限为0.2μg/mL,测定频率达60次/h,浓度为10μg/mL的试样7次测定的相对标准偏差为0.25%,在4～100μg/mL的浓度范围内严格遵守比尔定律,并用于市售维生素K3针剂含量的测定,结果与药典方法一致.

A flow injection spectrophotometric approach for determination of vitamin K3 was developed. A 250 μL aqueous sample solution of MSB was delivered by a water carrier to be merged and reacted with a dimethylamine solution(33%) in a coiled reactor made of a 100 cm×0.5mm PTFE tubing. The absorbance of the produced violet red complex compound was online measured at 510 nm. A detection limit of 0.2 μg/mL was achieved at the sampling frequency of 60/h, and determinations of a test solution containing 10 μg/mL vitamine K3 gave a RSD of 0.25%. Linear calibration curve was observed in the vitamine K3 concentration range of 4100 μg/mL. The developed method was applied to the vitamine K3 content in injection. The analytical results were in good agreement with that abtained by China Pharmacopoeia.