丙酸氟替卡松原料及其鼻喷雾剂中丙酸氟替卡松的含量和有关物质UPLC-MS/MS研究  

Determination of fluticasone propionate in raw materials and nasal sprays by UPLC-MS/MS

作　　者：陈忠兰 张雅军[1] 孙会敏[1] 王瑾[1] 吴先富[1] CHEN Zhong-an;ZHANG Ya-jun;SUN Hui-min;WANG Jin;WU Xian-fu(National Institutes for Food and Drug Control,Beijing 102629,China)

机构地区：[1]中国食品药品检定研究院,北京102629

出　　处：《中国新药杂志》2024年第3期301-306,共6页Chinese Journal of New Drugs

摘　　要：目的:建立UPLC法测定丙酸氟替卡松原料及鼻喷雾剂中丙酸氟替卡松的含量,并利用UPLC-MS/MS法对丙酸氟替卡松杂质进行分析研究。方法:采用HALO 90A,C_(18)色谱柱(100 mm×2.1 mm,2.7μm),流动相为乙腈-0.1%甲酸(含0.1%乙酸铵)溶液,梯度洗脱,流速0.3 mL·min^(-1),柱温40℃,检测波长239 nm。MS采用电喷雾离子(ESI)源,选择正离子模式检测,利用UPLC-MS/MS法对丙酸氟替卡松的杂质进行定性鉴别。结果:丙酸氟替卡松主成分色谱峰与各杂质之间分离良好,丙酸氟替卡松质量浓度在0.5~50.0μg·mL^(-1)范围内与峰面积呈良好的线性关系(R^(2)=0.9998),丙酸氟替卡松鼻喷雾剂的平均回收率为95.51%,RSD为1.59%(n=9),测得丙酸氟替卡松原料中丙酸氟替卡松的含量为99.54%,测得3批丙酸氟替卡松鼻喷雾剂含量为标示量的96.69%,98.32%,96.00%。结论:该方法快速、简便、灵敏,可用于丙酸氟替卡松及其鼻喷雾剂中丙酸氟替卡松的含量测定以及杂质的定性鉴别。Objective:To establish a UPLC method for the determination of fluticasone propionate in fluticasone propionate raw materials and nasal sprays,which can be used to qualitatively identify the impurities of fluticasone propionate.Methods:The analytes were separated on a HALO 90 A,C_(18) column(100 mm×2.1 mm,2.7μm)using a gradient elution with the mobile phase of acetonitrile-0.1%formic acid(containing 0.1%ammonium acetate).The flow rate was 0.3 mL·min^(-1),the column temperature was 40℃,and the detection wavelength was 239 nm.The impurities of fluticasone propionate were qualitatively identified by UPLC-MS/MS under an ESI positive mode.Results:The chromatographic peak for the principal component of fluticasone propionate was well separated from each impurity.The linearity range of fluticasone propionate was 0.5~50.0μg·mL^(-1)(R^(2)=0.9998),and the recovery of fluticasone propionate nasal spray was 95.51%(RSD=1.59%,n=9).The percentage of fluticasone propionate in the raw material was 99.54%,the percentage of labeled amount of three batches of fluticasone propionate nasal spray were 96.69%,98.32%and 96.00%,respectively.Conclusion:The method,

关 键 词：UPLC 丙酸氟替卡松 鼻喷雾剂 含量测定 定性鉴别 

分 类 号：R917[医药卫生—药物分析学]