摘要
Abstract
Objective To establish a liquid chromatographic-tandem mass spectrometric method for the determination of fluoxetine in human plasma. Methods The chromatographic condition: pre-column: guard column ( 4. 7 mm × 3. 0 mm ); analytical column: Allure C18 ( 50 mm × 4. 6 mm, 5 μm );the mobile phase was methanol-2 mmol/L ammonium acetate plus 5% formic acid solution ( 70:30, v/ v );the flow rate:0. 5 mL/min;the injection volume:10 μL;the column temperature:20 ℃. The mass spectrum condition:iron source was at-mospheric pressure chemical ionization ( ESI );the spray voltage ( IS ) was 4 500 V;the nebulization temperature was 550 ℃;the nebuliza-tion gas NEB ( gas 1 ) was 40 L/min;the curtain gas CUR was 20 L/min;the collision gas CAD was 5 L/min;the auxiliary gas AUX ( gas 2 ) was 40 L/min; the detection mode was cation ion multiple reaction monitoring ( MRM ) , the ion reaction for the quantitative analysis was m/ z:310. 3→148. 2 ( fluoxetine ) and m/ z:316. 1→270. 0 ( internal standard, clonazepam ) , the collision induction disaggrega-tion ( CID ) voltage was 13 V ( fluoxetine ) and 35 V ( clonazepam ) . Results The linear relation was good in the concentration range 0. 3-25. 0 ng/mL for fluoxetine ( r=0. 999 4-0. 999 9 ) , the lowest quantitative concentration was 0. 3 ng/mL. The relative recovery rate was 96. 7% -105. 7%. the intra-day and inter-day precision RSD < 10%. Conclusion The developed method is highly specific, accurate and sensitive, its sample processing procedure is simple and suitable for pharmacokinetic study of fluoxetine in human plasma.关键词
氟西汀/质谱/检测/药代动力学Key words
fluoxetine/mass spectrum/determination/pharmacokinetics分类
医药卫生