小儿复方吐根合剂枸橼酸钾含量测定方法的改进

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小儿复方吐根合剂为医院常用的儿科制剂,收载于浙江省历次制剂规范,其处方组成;枸橼酸钾150g,吐根糖浆150ml,单糖浆100ml,水加至1000ml。规范中对枸橼酸钾含量测定以橙黄Ⅳ作指示剂中和法测定含量,终点观察不明显。我们参照文献方法,改用比色法,并作了回收试验,认为该法简便准确,符合医院制剂快检要求。 1 仪器和试药 752紫外光栅分光光度计(上海第三分析仪器厂);麝香草酚蓝指示液;枸橼酸钾对照液(精密称取105℃干燥恒重的枸橼酸钾适量,加水精密配制使成每毫升含枸橼酸钾0.15g);0.5mol/L盐酸液。 2 测定方法 精密量取样品1ml两份及枸橼酸钾对照液1ml一份,分别置于25ml量瓶,各精密加入麝香草酚蓝指示液1ml,样品液分别精密加入0.5mol/L盐酸液2.77ml±5%(即甲液2.63ml,乙液2.91ml),对照液精密加入0.5mol/L盐酸液2.77ml,加水至刻度,摇匀,置1cm比色皿中,以水作空白,在波长544nm处测定吸收度,按下式求等当点时消耗0.5mol/L盐酸液毫升数(V_2)。 Pediatric compound spit root mixture for the hospital commonly used in pediatric preparations, contained in Zhejiang Province, the previous preparation specifications, the composition of the prescription; potassium citrate 150g, Iodine syrup 150ml, single syrup 100ml, water to 1000ml. The specification of potassium citrate content was determined by the method of orange yellow indicator neutralization method, the end point was not obvious. We refer to the literature method, the use of colorimetric method, and made a recovery test, that the method is simple and accurate, in line with the requirements of hospital preparations fast inspection. 1 instrument and reagent 752 UV grating spectrophotometer (Shanghai Third Analytical Instrument Factory); thymol blue indicator solution; potassium citrate control solution (accurately weighed 105 ℃ constant dry weight of potassium citrate, add water Precision preparation to make per ml of potassium citrate 0.15g); 0.5mol / L hydrochloric acid solution. 2 Determination of precise amount of sample 1ml two copies of citric acid and a control solution 1ml, respectively, placed in 25ml volumetric flask, the precise addition of thymol blue indicator solution 1ml, respectively, the sample solution were added precision 0.5mol / L hydrochloric acid solution 2.77ml ± 5% (ie A liquid 2.63ml, B liquid 2.91ml), the control solution was added 0.5mol / L hydrochloric acid solution 2.77ml, add water to the mark, shake, set 1cm cuvette, with water as a blank, Determination of absorbance at a wavelength of 544nm, according to the following formula to wait at the point consumption of 0.5mol / L hydrochloric acid ml (V_2).
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