title: Combination of a sub-3 μm superficially porous particle packed column with charged aerosol detection for the simple and sensitive measurement of nine macrolides in human urine.
abstract: Due to the lack of chromophores in many macrolides, analytical methods based on mass spectrometry and electrochemical detection coupled to liquid chromatography have been suggested to be suitable for the quantification of macrolides in complex matrices. In this study, a simple and sensitive analytical method was established for the simultaneous measurement of nine macrolides in human urine by combining a sub-3 μm superficially porous particle packed column with charged aerosol detection. After thorough investigation of various sample preparation methods, including two liquid-liquid extraction methods and four solid-phase extraction methods, HLB solid-phase extraction was selected and further optimized. Absolute recovery of the optimized sample preparation method ranged from 99.5-110.2%, indicating its very high extraction/clean-up efficiency. For chromatography, parameters influencing macrolide separation were systematically optimized, and the resulting conditions allowed baseline separation of nine macrolides within 24 min using a very simple mobile phase. The established method was validated for linearity, limit of detection, limit of quantification, absolute recovery, and precision. Based on its limit of detection (0.025-0.100 μg/mL), the method had similar or greater sensitivity than most methods based on electrochemical detection. It was found that the current method was appropriate for application to real human urine samples after drug administration.
authors.affiliation: College of Pharmacy, Seoul National University, Seoul, Korea.
authors.forename: Shaodong
authors.initials: S
authors.lastname: Jia
authors.forename: In Gi
authors.initials: IG
authors.lastname: Song
authors.forename: Kyung Min
authors.initials: KM
authors.lastname: Jeong
authors.forename: Jing
authors.initials: J
authors.lastname: Li
authors.forename: Jeong Hill
authors.initials: JH
authors.lastname: Park
authors.forename: Jeongmi
authors.initials: J
authors.lastname: Lee
authors.forename: Sung Won
authors.initials: SW
authors.lastname: Kwon
mesh_terms: D000336:Aerosols; D002851:Chromatography, High Pressure Liquid / Q000295:instrumentation / Q000379:methods*; D006801:Humans; D057230:Limit of Detection; D018942:Macrolides / Q000652:urine*; D012015:Reference Standards; D053719:Tandem Mass Spectrometry
chemical_list: D000336:Aerosols; D018942:Macrolides
keywords: Charged aerosol detection; Macrolides; Solid-phase extraction; Superficially porous particles; Urine analysis