摘要
目的建立硫酸庆大霉素滴眼液中8种抗氧剂含量的HPLC测定方法,考察包材中抗氧剂向药液的迁移情况。方法采用Inertsil ODS-3色谱柱(4.6 mm×100 mm,3μm);检测波长:200 nm;流速:1.0 mL/min;柱温:35℃;进样量:10μL;流动相为水-乙腈,梯度洗脱。采用正己烷对样品中的抗氧剂进行提取,建立硫酸庆大霉素滴眼液中抗氧剂BHA、抗氧剂XH-245、抗氧剂BHT、抗氧剂3114、抗氧剂1010、抗氧剂330、抗氧剂1076和抗氧剂168含量的测定方法,并进行方法学验证,同时测定了企业提供的原辅料和包材中8种抗氧剂的含量,并对制剂进行了影响因素考察试验。结果8种抗氧剂之间的分离度良好,均在0.3~30μg/mL浓度范围内线性关系良好(r≥0.9994)。方法精密度、重复性、回收率、稳定性均符合有关规定。硫酸庆大霉素滴眼液、原辅料中均未检出8种抗氧剂,包材中仅检出抗氧剂BHT,影响因素试验表明样品中8种抗氧剂的迁移不受高温、高湿和强光照射的影响,表明本品由包材中抗氧剂迁移带来的安全风险较低。结论所建立的方法灵敏、快速、准确、重复性好,提取方法简单,可用于硫酸庆大霉素滴眼液中8种抗氧剂迁移情况的监测和溯源。
Objective To establish an HPLC method for determining the content of eight antioxidants in gentamicin sulfate eye drops,and study the migration of antioxidants from plastic packaging materials to eye drops.Methods HPLC was performed on an Inertsil ODS-3 column(4.6 mm×100 mm,3μm)with the mobile phase of acetonitrile-water(gradient elution).The flow rate was 1.0 mL/min,the detection wavelength was 200 nm,the column temperature was maintained at 30℃,and the sample volume was 10μL.The antioxidant in the sample was extracted with n-hexane.The HPLC method was set up to determine the contents of antioxidant BHA,XH-245,BHT,3114,1010,330,1076,and 168.At the same time,the contents of eight antioxidants in the preparations,raw and auxiliary materials,and packaging materials provided by the enterprise were determined,and the influencing factors of the preparations were investigated.Results The eight antioxidants were well separated,which showed good linear relationship in the concentration range of 0.3~30μg/mL(r≥0.9994).The specificity,the precision,the accuracy,and the robustness were good.Conclusions The method is sensitive,rapid and accurate with good repeatability,which can be used to evaluate the migration of antioxidants from packaging materials and containers to gentamicin sulfate eye drops.
作者
卢玉凤
张振中
Lu Yu-feng;Zhang Zhen-zhong(Zhengzhou University,Zhengzhou 450001;Institute for Food and Drug Control of Henan Province,Zhengzhou 450018)
出处
《中国抗生素杂志》
CAS
CSCD
北大核心
2022年第11期1182-1187,共6页
Chinese Journal of Antibiotics
关键词
高效液相色谱法
硫酸庆大霉素滴眼液
抗氧剂
原辅料
包材
HPLC
Gentamicin sulfate eye drops
Antioxidant
Raw and auxiliary materials
Packaging materials
