摘要
目的:建立同时测定药用软膏管中12种光引发剂的分析方法。方法:将剪碎的药用软膏管于乙腈中超声30 min,利用超高效合相色谱技术,采用ACQUITY UPC2 CSHTM Fluoro-Phenyl(100 mm×3.0 mm,1.7μm)色谱柱,以超临界CO_(2)为主要流动相,同时以甲醇为改性剂进行梯度洗脱,流速1.5 mL·min^(-1),系统背压13.79 MPa,柱温50℃,进样体积1μL,采用二极管阵列检测器(PDA)。结果:12种光引发剂可在3 min内实现分离检测,各化合物线性关系在2~100μg·mL^(-1)内良好,相关系数r均>0.999;平均加标回收率范围为85.7%~117.2%,RSD(n=6)为0.40%~4.8%;对6批药用软膏管样品进行检测,主要检测到光引发剂DETX。结论:该法快速、环保、简单、准确,可用于药用软膏管中光引发剂的快速检测。
Objective:To develop a method for the rapid determination of 12 photoinitiators in medicinal ointment tubes.Methods:Shredded medicinal ointment tubes were extracted by acetonitrile.Ultrasound was used to ultrasondiate these samples for 30 min.Ultra-performance convergence chromatography was adopted.The determination was performed on ACQUITY UPC2 CSHTM Fluoro-Phenyl(100 mm×3.0 mm,1.7μm),supercritical carbon dioxide fluid and methanol were used as gradient elution and the flow rate of 1.5 mL·min^(-1).The automatic back pressure regulator was 13.79 MPa.The column temperature was 50℃.The injection volume was 1μL.The photodiode array detector was used.Results:The full baseline separation of the 12 photoinitiators were achieved in 3 min.12 photoinitiators had good linear relationships within the ranges of 2-100μg·mL^(-1),respectively.And the correlation coefficients(r)was above 0.999.The average recoveries were 85.7%-117.2%,and RSDs were 0.40%-4.8%.The results showed the DETX was mainly detected in the 6 batches of medicinal ointment tubes.Conclusion:This method is rapid,environmentally friendly,simple,accurate,which can be used for the rapid determination of photoinitiators in medicinal ointment tubes.
作者
曹运姣
刘晨曦
陈雷霖
陈晓莉
付蒙
胡敏
尚悦
CAO Yun-jiao;LIU Chen-xi;CHEN Lei-lin;CHEN Xiao-li;FU Meng;HU Min;SHANG Yue(School of Pharmacy,Hubei University of Chinese Medicine,Wuhan 430065,China;NMPA Key Laboratory of Traditional Chinese Medicine,Hubei Institute for Drug Control,Hubei Engineering Research Center for Drug Quality Control,Wuhan 430075,China;Chinese Pharmacopoeia Commission,Beijing 100061,China)
出处
《药物分析杂志》
北大核心
2025年第4期718-726,共9页
Chinese Journal of Pharmaceutical Analysis
基金
湖北省药品监督检验研究院中青年科研基金资助项目(2022YN004)。
关键词
超高效合相色谱法
超临界CO_(2)
药用软膏管
光引发剂
环保
ultra-performance convergence chromatography
supercritical CO_(2)
medicinal ointment tubes
photoinitiators
environmentally friendly
作者简介
第一作者:曹运姣,Tel:15102795624,E-mail:1483592824@qq.com;通信作者:胡敏,Tel:(027)87705232,E-mail:humin@hubyjs.org.cn;通信作者:付蒙,Tel:(027)87705260,E-mail:fumeng@hubyjs.org.cn。
