Development and full validation of a sensitive quantitative assay for the determination of clemastine in human plasma by liquid chromatography-tandem mass spectrometry.
A sensitive high-performance liquid chromatography-tandem mass spectrometry (LC/MS/MS) method was developed and validated for the determination of clemastine in human plasma. After having been extracted from plasma samples by ethyl acetate, clemastine and internal standard, diphenhydramine, were separated on a C(18) column. Detection was performed on Thermo Finnigan TSQ Quantum triple quadrupole mass spectrometer by selected reaction monitoring (SRM) mode via electrospray ionization (ESI) source. The method was linear in the concentration range of 5.0-1000.0 pg/ml for clemastine. The intra- and inter-day precisions were within 13.4% and the deviations were between -1.1% and 5.6%. The fully validated LC/ESI-MS/MS method has been successfully applied to the preliminary pharmacokinetic study in healthy male Chinese volunteers.
Xie
Zhiyong
Z
Laboratory of Pharmaceutical Analysis & Quality Assessment, School of Pharmaceutical Sciences, Sun Yat-sen University, 74 Zhongshan Road II, Guangzhou 510080, China.
Liao
Qiongfeng
Q
Li
Zuojun
Z
Zhu
Chenchen
C
Zeng
Yuaner
Y
Liu
Shikun
S
D000082:Acetaminophen / Q000032:analysis; D000328:Adult; D002138:Calibration; D002851:Chromatography, High Pressure Liquid; D002974:Clemastine / Q000097:blood* / Q000493:pharmacokinetics; D004338:Drug Combinations; D004355:Drug Stability; D004809:Ephedrine / Q000032:analysis; D005615:Freezing; D006634:Histamine H1 Antagonists / Q000097:blood* / Q000493:pharmacokinetics; D006801:Humans; D008297:Male; D011786:Quality Control; D012015:Reference Standards; D015203:Reproducibility of Results; D012996:Solutions; D021241:Spectrometry, Mass, Electrospray Ionization; D053719:Tandem Mass Spectrometry; D013696:Temperature
D004338:Drug Combinations; D006634:Histamine H1 Antagonists; D012996:Solutions; D000082:Acetaminophen; D002974:Clemastine; D004809:Ephedrine