氨基糖苷类抗生素中硫酸盐的两种测定方法比较 - 中国药品标准杂志.doc

氨基糖苷类抗生素中硫酸盐的比较 姚永青，刘英*（河南省食品药品检验所，郑州450003） 摘要 目的：比较并氨基糖苷类抗生素中硫酸盐的两种测定方法。方法：用对抗生素中的硫酸盐测定HPLC-ELSD法色谱柱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：进行两种方法配对检验，无显著性差异。结论：滴定法为经典分析方法，成本低廉，但需要始终保持液pH值11，操作繁琐HPLC-ELSD法测定三种抗生素中专属性、准确、易操作，关键词：滴定法；高效液相蒸发光散射检测器法；硫酸盐；氨基糖苷类抗生素中图分类号：R921.2 文献标志码：A Comparison of Two Methods for Determination of the Sulfate in Aminoglycoside and Polypeptide Antibiotics Yao Yongqing，L Ying*（Henan Institute for Food and Drug Control，Zhengzhou 450003） Abstract Objective: To ompare 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，P0.05). 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. Key words: Complexometric titration；HPLC-ELSD；Sulfate；Ami