摘要
目的建立同时测定药用复合软膏管中10种光引发剂的定量分析方法。方法对剪碎的药用复合软膏管超声30 min,利用GC-MS技术对样品进行检测。色谱柱为DB17-MS毛细管色谱柱(0.25 mm×30 m,0.25μm),进样口:300℃,流速:1 mL·min^(-1),柱温:初始70℃,保持0.5 min,再以10℃·min^(-1)升至300℃,保持7 min。进样类型:液体进样,进样体积:1μL。离子源:EI,温度:290℃,电压:70 eV,溶剂延迟5 min。结果10种光引发剂分离度良好,在浓度0.05~10μg·mL^(-1)内线性关系良好,相关系数r^(2)在0.9945~0.9988之间;平均回收率(n=9)在84.9%~94.6%之间,相对标准偏差(RSD)在3.9%~8.5%之间,检测限在0.2~0.5μg·g^(-1),定量限在0.5~1.0μg·g^(-1)。结论该方法经方法学验证,操作简便,方法准确性、重复性好,可用于复合软膏管中10种光引发剂的筛查。
OBJECTIVE To develop a quantitative analytical method for simultaneous determination of 10 photoinitiators in medicinal compound ointment tubes.METHODS Ultrasound was used to ultrasonicate the shredded medicinal compound ointment tube for 30 min,and the samples were detected by GC-MS technology.Chromatographic column was DB17-MS capillary column(0.25 mm×30 m,0.25μm),injection port:300℃,flow rate:1 mL·min^(-1),column temperature:initial 70℃,hold for 0.5 min,and then rise at 10℃·min^(-1) to 300℃,keeping for 7 min.Injection type:liquid injection,injection volume:1μL.Ion source:EI,temperature:290℃,voltage:70 eV,solvent delay 5 min.RESULTS The 10 kinds of photoinitiators were well separated,with good linear relationship in the concentration range of 0.05-10μg·mL^(-1).The correlation coefficient r^(2) was between 0.9945-0.9988;the average recoveries(n=9)were 84.9%-94.6%,and the RSDs were between 3.9% and 8.5%.The limits of detection were between 0.2 and 0.5μg·mL^(-1),and the limits of quantification were between 0.5 and 1.0μg·mL^(-1).CONCLUSION This method is validated to have good method accuracy and reproducibility,is easy to operate,and can be used for the determination of 10 photoinitiators in compound ointment tubes.
作者
汪元亮
常亮
辜倩
熊马剑
朱碧君
赵霞
WANG Yuanliang;CHANG Liang;GU Qian;Xiong Majian;ZHU Bijun;ZHAO Xia(Jiangxi Institute for Drug Control,NMPA Key Laboratory for Quality Evaluation of Traditional Chinese Patent Medicine,Jiangxi Province Engineering Research Center of Drug and Medical Device Quality,Nanchang 330029,China;Jiangxi University of Traditional Chinese Medicine,Nanchang 330004,China;National Institutes for Food and Drug Control,Beijing 100050,China)
出处
《中国药学杂志》
CAS
CSCD
北大核心
2023年第23期2120-2126,共7页
Chinese Pharmaceutical Journal
基金
江西省药品监督管理局科研项目资助(2021KY31)
中国食品药品检定研究院中青年发展研究基金项目资助(2023C6)。
关键词
光引发剂
气质联用法
药用软膏管
药包材
photoinitiator
GC-MS
medicinal ointment tube
drug packaging material
