16 / 19
allied
academies
Page 39
Journal of Systems Biology & Proteome Research
|
Volume 2
J u n e 2 5 - 2 7 , 2 0 1 8 | D u b l i n , I r e l a n d
MASS SPECTROMETRY
AND PROTEOMICS
International Conference on
Aymen K AL- Suwailem, J Syst Biol Proteome Res 2018, Volume 2
HPLC-FLUORESCENCE METHOD FOR
THE ENANTIOSELECTIVE ANALYSIS OF
PROPRANOLOL IN RAT SERUM USING
IMMOBILIZED POLYSACCHARIDE-
BASED CHIRAL STATIONARY PHASE
Aymen K AL- Suwailem
King Saud University, Saudi Arabia
T
stereoselective high-performance liquid chromatographic (HPLC) meth-
od was developed and validated to determine S-(-)- and R-(+)-propranolol
in rat serum. Enantiomeric resolution was achieved on cellulose tris(3,5-di-
methylphenylcarbamate) immobilized onto spherical porous silica chiral sta-
tionary phase (CSP) known as Chiralpak IB. A simple analytical method was
validated using a mobile phase consisted of n-hexane-ethanol-triethylamine
(95:5:0.4%, v/v/v) at a flow rate of 0.6 mL min
-1
and fluorescence detection
set at excitation/emission wavelengths 290/375 nm. The calibration curves
were linear over the range of 10–400 ng mL
-1
(R = 0.999) for each enantio-
mer with a detection limit of 3 ng mL
-1
. The proposed method was validated
in compliance with ICH guidelines in terms of linearity, accuracy, precision,
limits of detection and quantitation, and other aspects of analytical valida-
tion. Actual quantification could be made for propranolol isomers in serum
obtained from rats that had been intraperitoneally (i.p.) administered a single
dose of the drug. The proposed method established in this study is simple
and sensitive enough to be adopted in the fields of clinical and forensic toxi-
cology. Molecular modeling studies including energy minimization and dock-
ing studies were first performed to illustrate the mechanism by which the
active enantiomer binds to the β-adrenergic receptor and second to find a
suitable interpretation of how both enantiomers are interacting with cellulose
tris(3,5-dimethylphenylcarbamate) CSP during the process of resolution. The
latter interaction was demonstrated by calculating the binding affinities and
interaction distances between propranolol enantiomers and chiral selector.
Chirality 00:000–000, 2014.
Key Words:
propranolol; enantioselective; Chiralpak IB; HPLC-FD; molec-
ular modeling.
aymen_4120@hotmail.com