高效液相色谱法测定异烟酸辛酰肼含量
Isonicotinic acid octylidene-hydrazideassay by HPLC
吴林静 1马成 2郭梦琴 1黄郑炜 1黄莹 1吴传斌 1潘昕2
作者信息
- 1. 暨南大学药学院,广州 511436
- 2. 中山大学药学院,广州 510006
- 折叠
摘要
目的:异烟肼及其衍生物作为治疗肺结核的一线药物,其含量测定在药物的研发及应用中至关重要.然而,异烟肼的含量测定方法虽常有报道,但是针对异烟肼衍生物的含量测定方法却鲜有报道.因此本研究构建一种适用于测定异烟酸辛酰肼(INH-CHO)的反相高效液相色谱法(reverse-phase high performance liquid chromatography,RP-HPLC),用于INH-CHO的含量检测.方法:采用Capcell Pak C18 MG Ⅱ S5 色谱柱,柱温为30℃,以pH=6.0磷酸盐缓冲液:甲醇=30:70为流动相进行洗脱,流速为1 mL/min,进样0.02 mL,在262 nm处检测,考察该方法学的线性关系、精密度、准确度及定量限.结果:INH-CHO的保留时间为 9.2 min,在 1～240 μg/mL、0.1～1 μg/mL浓度范围内都具有较好的线性关系(R²＞0.999 0),在该色谱条件下测定INH-CHO的日内精密度、日间精密度、准确度较好,定量限为 0.1 μg/mL.结论:在实验浓度范围内,该方法线性良好、操作简便、结果精确、可重现,适用于INH-CHO的含量检测.
Abstract
Objective:Isoniazid and its derivatives are the first-line drugs for the treatment of tuberculosis,and their content determination is crucial in the development and application of drugs.However,although methods for determining the content of isoniazid are reported,there are few reports on methods for determining the content of isoniazid derivatives.Therefore,in this study,a reversed-phase high performance liquid chromatography(RP-HPLC)method suitable for the determination of isonicotinic acid octanoyl hydrazide(INH-CHO)was constructed for the content detection of INH-CHO.Methods:Capcell Pak C18 MG Ⅱ S5 chromatographic column was used,the column temperature was 30℃,the mobile phase was pH=6.0 phosphate buffer:methanol=30:70 for elution,the flow rate was 1 mL/min,and the injection volume was 0.02 mL,the detecting wavelength was 262 nm.Through the above method,the linear relationship,precision,accuracy and limit of quantification of the methodology were investigated.Results:The retention time of INH-CHO was 9.2 min,and there was a good linear relationship in the concentration range of 1-240 μg/mL and 0.1-1 μg/mL.The intra-day precision,inter-day precision and accuracy were satisfied,and the limit of quantification was 0.1 μg/mL.Conclusion:In the experimental concentration range,the method had good linearity,simple operation,accurate and reproducible results,and was suitable for the determination of INH-CHO content.
关键词
药剂学/反相高效液相色谱法/INH-CHO/含量测定Key words
pharmaceutics/reverse high performance liquid chromatography/INH-CHO/content quantification引用本文复制引用
基金项目
中央高校基本科研业务费专项(21621012)
国家自然科学基金青年科学基金(82104070)
出版年
2024
NETL
NSTL
万方数据