文章摘要
姚永青,刘英.氨基糖苷类及多肽类抗生素中硫酸盐的两种测定方法比较[J].中国药品标准,2017,18(1):19-24
氨基糖苷类及多肽类抗生素中硫酸盐的两种测定方法比较
Comparison of Two Methods for Determination of the Sulfate in Aminoglycoside and Polypeptide Antibiotics
投稿时间:2016-08-18  修订日期:2017-01-19
DOI:
中文关键词: 络合滴定法  高效液相蒸发光散射检测器法  硫酸盐  氨基糖苷类抗生素  多肽类抗生素
英文关键词: Complexometric titration  HPLC-ELSD  Sulfate  Aminoglycoside antibiotics  Polypeptide antibiotic
基金项目:
作者单位E-mail
姚永青* 河南省食品药品检验所 yaoyongqing.1984@163.com 
刘英* 河南省食品药品检验所 yaoyongqing.1984@163.com 
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中文摘要:
      的:比较并探讨氨基糖苷类及多肽类抗生素中硫酸盐的两种测定方法。方法:用络合滴定法和HPLC-ELSD法分别对三种抗生素中的硫酸盐进行测定;HPLC-ELSD法色谱柱为Grace Apollo C18(4.6 mm×250 mm,5 μm),流动相为0.2 mol﹒L-1三氟乙酸溶液-甲醇柱温35 ℃,进样量20 μl。结果:进行两种方法配对t检验分析,t=0.436,P>0.05,结果无显著性差异。结论:络合滴定法为经典分析方法,成本低廉,但需要始终保持待测液pH值11,且调节pH时应注意避免反应离子及待测离子的损失,操作繁琐,耗时较长,在滴定过程中产生的白色沉淀对终点的判断有影响,主观性较强;而HPLC-ELSD法测定三种抗生素中的硫酸盐,专属性、准确度、精密度均良好 ,方法易操作,克服了滴定法判断终点的主观性,能更为准确快捷地测定氨基糖苷类及多肽类抗生素中硫酸盐的含量。
英文摘要:
      Objective: To compare and discuss the two methods for determination of the sulfate in Aminoglycoside and Polypeptide antibiotics. Methods: The complexometric titration and HPLC-ELSD methods were used for determination of the sulfate in 3 antibiotics.For HPLC-ELSD method, Grace Apollo C18(4.6 mm×250 mm, 5 μm) was used, the mobile phase was 0.2mol?L-1 trifluoroacetic acid solution- methanol,the column temperature was set at 35 ℃, and the injection volume was 20 μL. Results: The paired t test was used for comparison of two methods, and no significant difference was observed (t=0.436,P>0.05). Conclusion: Complexometric titration belongs to the classical method with low costs, but the pH value of the test solution need be kept as 11 in the titration process. The loss of reaction ions and the test ions should be avoided when adjusting pH, and the operation is complicated and time-consuming. Moreover, the white precipitation produced in the process of titration may interfere with the judgement of titration endpoint. This method has a strong subjectivity. The HPLC-ELSD method for determination of the sulfate in three kinds of antibiotics has the good specificity, precision and accurate which is operated conveniently and can overcome the subjectivity of titration endpoint judgement. It can be used to determine the sulfate in Aminoglycoside antibiotics and Polypeptide antibiotics accurately and quickly.
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