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.doc

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 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。 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 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 ， Liu Ying * （ Henan Institute for Food and Drug Control ，Zhengzhou 450003） Abstract 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