UPLC-QTOF-MS/MS快速筛查抗鼻炎类制剂中非法添加3种咪唑啉类化合物

Rapid Screening of 3 Imidazoline Compounds Illegally Added in Anti-rhinitis Pharmaceutics by UPLC-QTOF-MS/MS

目的:建立抗鼻炎类制剂中3种咪唑啉类化合物(盐酸萘甲唑啉、盐酸羟甲唑啉、盐酸赛洛唑啉)的超高效液相色谱四极杆飞行时间质谱的快速筛查方法。方法:滴鼻液、鼻炎喷剂、鼻炎膏等不同类型样品经提取过滤后,通过AgilentZORBAXExtendC18色谱柱(2.1mm×50mm,1.8μm)在5min内完成有效分离后,采用电喷雾四级杆飞行时间质谱进行筛查分析。结果:3种化合物的检出限为10.0~26.3ng·mL^-1,在低、中、高3个浓度的平均加标回收率为92.6%~104.0%,相对标准偏差1.68%~4.65%。结论:该方法快速、简便、准确,为抗鼻炎类制剂的高通量快速筛查提供了可靠实用的技术手段。

Objective: A comprehensive analytical method using ultra performance liquid chromatography coupled with quadrupole time-of-flight mass spectrometry was developed for screening rapidly of 3 imidazoline compounds (naphazoline hydrochloride, oxymetazoline hydrochloride, xylometazoline hydrochloride) added in anti-rhinitis pharmaceutics. Methods: After nasal drops, nasenspray and nasal pastewere were extracted with solvents and filtered, the solutions would be separated on a Agilent ZORBAX Extend C18 column(2.1 mm×50 mm,1.8 μm)and screened analysis carried out by electrospray ionization quadrupole time-of-flight mass spectrometry (Q-TOF/MS) with in 5 min. Results : The limits of detection for 3 compounds were from10.0 ng·mL^-1 to 26.3 ng·mL^-1 , the mean recoveries at three spiked levels was from 92.6% to 104.0%, and the relative standard deviations were from 1.68% to 4.65%. Conclusion : The method is rapid, simple and accurate, and provides a reliable and effective technique for high-throughput screening of anti-rhinitis preparations.