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- Title
Indirect enantioseparation of fluoxetine in mouse serum by derivatization with 1 R-(-)-menthyl chloroformate followed by ultra high performance liquid chromatography and quadrupole time-of-flight mass spectrometry.
- Authors
Zhao, Jing; Jin, Yan; Shin, Yujin; Jeong, Kyung Min; Lee, Jeongmi
- Abstract
Here we describe a simple and sensitive analytical method for the enantioselective quantification of fluoxetine in mouse serum using ultra high performance liquid chromatography with quadrupole time-of-flight mass spectrometry. The sample preparation method included a simple deproteinization with acetonitrile in 50 μL of serum, followed by derivatization of the extracts in 50 μL of 2 mM 1 R-(-)-menthyl chloroformate at 45ºC for 55 min. These conditions were statistically optimized through response surface methodology using a central composite design. Under the optimized conditions, neither racemization nor kinetic resolution occurred. The derivatized diastereomers were readily resolved on a conventional sub-2 μm C18 column under a simple gradient elution of aqueous methanol containing 0.1% formic acid. The established method was validated and found to be linear, precise, and accurate over the concentration range of 5.0-1000.0 ng/mL for both R and S enantiomers ( r2 > 0.993). Stability tests of the prepared samples at three different concentration levels showed that the R- and S-fluoxetine derivatives were relatively stable for 48 h. No significant matrix effects were observed. Last, the developed method was successfully used for enantiomeric analysis of real serum samples collected at a number of time points from mice administered with racemic fluoxetine.
- Subjects
ENANTIOSELECTIVE catalysis; FLUOXETINE; LIQUID chromatography; TIME-of-flight mass spectrometry; RESPONSE surfaces (Statistics)
- Publication
Journal of Separation Science, 2016, Vol 39, Issue 6, p1041
- ISSN
1615-9306
- Publication type
Article
- DOI
10.1002/jssc.201501163