络合滴定法测定复方钾钙镁溶液中氯化钙含量的方法学验证与不确定度分析
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摘要
目的:对络合滴定法测定复方钾钙镁溶液中氯化钙含量的方法进行方法学验证与不确定度分析。方法:采用乙二胺四乙酸(EDTA)滴定液0.05 mol/L滴定样品中氯化钙的含量,验证方法的适用范围、线性关系、准确度与精密度;通过绘制样品的分析测定流程图,分析不确定度的来源,计算方法的不确定度。结果:当氯化钾质量浓度在0.011 6～0.017 4 g/ml范围内时,络合滴定法消耗滴定液的体积与药物浓度有良好的线性关系;平均回收率为99.54%,精密度为0.39%。氯化钙的质量分数为1.51%,其扩展的不确定度为0.027 4%(k=2)。结论:络合滴定法测定复方钾钙镁溶液中氯化钙的含量,具有良好的准确度与精密度;该方法不确定度的主要来源为消耗滴定液的体积,适当增加样品取样量或者适当减小滴定液的浓度,从而增加消耗滴定液的体积,可以减小该方法的不确定度。本研究可为复方钾钙镁溶液及其同类产品含量测定的质量标准制定提供参考。
OBJECTIVE: To conduct methodology validation and uncertainty analysis on complexometry for the determination of calcium chloride in compound potassium, calcium and magnesium solution. METHOD: The content of calcium chloride in the sample was titrated with 0.05 mol/L of ethylenediaminetetraacetic acid(EDTA) titration solution, so as to validate its application range, linear relation, accuracy and precision; to analyze the source of uncertainty and calculate the uncertainty through drawing flow chart of plotting samples. RESULTS: When the concentration of potassium chloride was in the range of 0.011 6 g/ml-0.017 4 g/ml, the volume of titration solution consumed by the complexometry had a good linear relation with the drug concentration; the average recovery was 99.54%, precision was 0.39%. The mass fraction of calcium chloride was 1.51%, with the uncertainty of its expansion was 0.027 4%(k=2). CONCLUSIONS: The determination of calcium chloride in compound potassium, calcium and magnesium solution by complexometry has good accuracy and precision; the main source of its uncertainty is the volume of titration solution, by properly increasing the sample volume or reducing the concentration of titration solution, thereby increasing the volume of titration solution, the uncertainty of complexometry can be reduced. This study can provide reference for the formulation of quality standards for the determination of compound potassium, calcium and magnesium solution and its similar products.
OBJECTIVE: To conduct methodology validation and uncertainty analysis on complexometry for the determination of calcium chloride in compound potassium, calcium and magnesium solution. METHOD: The content of calcium chloride in the sample was titrated with 0.05 mol/L of ethylenediaminetetraacetic acid(EDTA) titration solution, so as to validate its application range, linear relation, accuracy and precision; to analyze the source of uncertainty and calculate the uncertainty through drawing flow chart of plotting samples. RESULTS: When the concentration of potassium chloride was in the range of 0.011 6 g/ml-0.017 4 g/ml, the volume of titration solution consumed by the complexometry had a good linear relation with the drug concentration; the average recovery was 99.54%, precision was 0.39%. The mass fraction of calcium chloride was 1.51%, with the uncertainty of its expansion was 0.027 4%(k=2). CONCLUSIONS: The determination of calcium chloride in compound potassium, calcium and magnesium solution by complexometry has good accuracy and precision; the main source of its uncertainty is the volume of titration solution, by properly increasing the sample volume or reducing the concentration of titration solution, thereby increasing the volume of titration solution, the uncertainty of complexometry can be reduced. This study can provide reference for the formulation of quality standards for the determination of compound potassium, calcium and magnesium solution and its similar products.
引文
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[16] 吴凯华,张相山,王国龙,等.浅谈量值传递和量值溯源的实施[J].计量与测试技术,2013,40(1):52-53.
[17] 夏黎明,王宏青.EDTA络合滴定钙镁方法的改进[J].精细化工中间体,1998,28(2):43-45.
[2] Han H.Measurement Uncertainty[M].Springer International Publishing,2016.
[3] 施昌彦.测量不确定度评定与表示指南[M].北京:中国计量出版社,2000.
[4] 李慎安.化学实验室测量不确定度[M].北京:化学工业出版社,2007.
[5] 中国实验室国家认可委员会.化学分析中不确定度的评估指南[M].北京:中国计量出版社,2002.
[6] 蔡慎,郑英丽,陈宝玲等.复方钾钙镁液中细菌内毒素检查法的可行性研究[J].中国药房,2010,21(21):1997-1998.
[7] 李云龙.中国药品检验标准操作规程[M].北京:中国医药科技出版社,2010.
[8] 陈华,王慧.关于线性回归法与单点外标法测量不确定度评估的初步探讨[J].药物分析杂志,2008,28(2):251-255.
[9] 林奎明.B类不确定度计算方法的探讨[J].计量技术,2000(3):52-54.
[10] 中华人民共和国国家计量检定规程JJG196-2006,常用玻璃量器[S].北京:中国计量出版社,2007:7-15.
[11] 张晓敏.EDTA滴定法测定石灰石中氧化钙含量不确定度的评定[J].山西化工.2015,15(3):34-37.
[12] 王也,裘国丽,黄华.络合滴定法测定葡萄糖酸钙含量的不确定度评定[J].海峡药学.2011,23(11):54-57.
[13] 程银宝,陈晓怀,王汉斌.基于精度理论的测量不确定度评定与分析[J].电子测量与仪器学报.2016,30(8):1175-1182.
[14] 臧慕文.分析测试不确定度的评定与表示[J].分析试验室,2005,24(11):74-79.
[15] 李发美.分析化学[M].5版.北京:人民卫生出版社,2011.
[16] 吴凯华,张相山,王国龙,等.浅谈量值传递和量值溯源的实施[J].计量与测试技术,2013,40(1):52-53.
[17] 夏黎明,王宏青.EDTA络合滴定钙镁方法的改进[J].精细化工中间体,1998,28(2):43-45.