摘要
目的完善曲尼司特滴眼液的质量标准。方法考察曲尼司特滴眼液的pH值。采用HPLC法测定样品中的有关物质和羟苯甲酯,采用C_(18)柱(250 mm×4.6 mm,5μm),流动相A为0.02 mol·L^(-1)磷酸二氢钾溶液(磷酸调pH2.0),流动相B为甲醇,梯度洗脱,检测波长为255 nm。结果曲尼司特滴眼液体系的pH值对羟苯甲酯的稳定性有重要影响。曲尼司特、对羟基苯甲酸、羟苯甲酯的线性范围分别为0.5860~146.5、0.0248~30.9474、0.0265~110.5μg·mL^(-1),r均为0.9999;对羟基苯甲酸相对曲尼司特的校正因子为0.36;曲尼司特、羟苯甲酯的检测限分别为219.7、3.68 ng·mL^(-1);羟苯甲酯的平均回收率为99.68%,RSD=0.78%。结论所用方法专属性强、重复性好、检测指标合理,可有效检出曲尼司特滴眼液的杂质,且便于控制羟苯甲酯的含量。适用于曲尼司特滴眼液的质量控制。
OBJECTIVE To improve the quality standard of Tranilast eye drops.METHODS The pH value of Tranilast eye drops was investigated.The related substances and methyl hydroxybenzoate were determined by HPLC.The determination of related substances and methyl hydroxybenzoate used a C_(18) column(250 mm×4.6 mm,5μm),with 0.02 mol·L^(-1) potassium dihydrogen phosphate solution(pH adjusted to 2.0 with phosphoric acid)as phase A and methanol as phase B for gradient elution.The detection wavelength was set at 255 nm.RESULTS The pH value of tranilast eye drops system had an important effect on the stability of methyl hydroxybenzoate.The linear ranges of Tranilast,p-hydroxybenzoic acid and methyl hydroxybenzoate were 0.5860-146.5μg·mL^(-1),0.0248-30.9474μg·mL^(-1) and 0.0265-110.5μg·mL^(-1),respectively.The regression coefficients were all 0.9999.The correction factor of p-hydroxybenzoic acid relative to tranilast was 0.36.The detection limits of Tranilast and methyl hydroxybenzoate were 219.7 ng·mL^(-1) and 3.68 ng·mL^(-1),respectively.The average recovery of methyl hydroxybenzoate was 99.68%with the RSD of 0.78%.CONCLUSION The quality standard has strong specificity,good repeatability and reasonable detection indicators,and can effectively detect the impurities in Tranilast eye drops and facilitate the control of the amount of methyl hydroxybenzoate.It can be used for the quality control of Tranilast eye drops.
作者
周明
李昌亮
李晓燕
李琦
ZHOU Ming;LI Changliang;LI Xiaoyan;LI Qi(Hunan Institute for Drug Control,Changsha,Hunan,410000 P.R.China;Hunan Center for Drug Evaluation,Changsha,Hunan,410000 P.R.China)
出处
《华西药学杂志》
CAS
CSCD
2022年第3期322-325,共4页
West China Journal of Pharmaceutical Sciences
基金
国家药品标准提高工作(化药)项目(编号:192)。
