Enantioseparation and Determination of Propranolol in Human Plasma on a New Derivatized β-Cyclodextrin Bonded Phase by HPLC
10.11895/j.issn.0253-3820.140102
- VernacularTitle:新型衍生化β-环糊精液相色谱键合相拆分和测定人体血浆中普萘洛尔对映体
- Author:
Rendan ZHOU
;
Laisheng LI
;
Biaoping CHENG
;
Guizhen NIE
;
Hongfu ZHANG
- Publication Type:Journal Article
- Keywords:
High performance liquid chromatography;
β-Cyclodextrin bonded SBA-15 chiral stationary phase;
Chiral separation;
β-Blockers;
Propranolol;
Plasma
- From:
Chinese Journal of Analytical Chemistry
2014;(7):1002-1009
- CountryChina
- Language:Chinese
-
Abstract:
A 6-azido-β-cyclodextrin was synthesized and derivatized with p-nitrophenyl isocyanate as chiral ligand. Following that the ligand was chemically bonded to mesoporous SBA-15 via a ‘Click Chemistry ’ reaction of the azido group with alkynyl group. A new p-nitrophenylcarbamoylatedβ-cyclodextrin bonded SBA-15 chiral stationary phase ( NPCSP ) for HPLC was obtained. The new stationary phase was first used to enantioseparate propranolol in human plasma under the polar organic solvent mode. The effects of methanol content , additive concentration of glacial acetic acid/triethylamine in mobile phase and the temperature on the enantioseparation were studied. The optimal chromatographic conditions were as follows: mobile phase was acetonitrile/methanol/glacial acetic acid/triethylamine (90:10:1. 25:2. 25, V/V), temperature 288 K, flow rate of 0. 5 mL/min, injection volume of 20 μL, detection wavelength at 290 nm. The resolution was 2. 04 with a short run time (< 15 min) under the above conditions. The composition of propranolol in plasma was quantitatively measured by HPLC-MS selected ion monitoring mode ( [ M +H ]+ m/z 260 . 10 ) with hydrochlorothiazide as internal standard. And linear range was 2. 5-250 μg/L and with a good linear relationship. The detection limit was 1 μg/L according to S/N=3. The experimental results showed that the chiral stationary phase exhibited excellent chiral separation ability to propranolol and the analysis method for propranolol in plasma was sensitive, accurate, simple and fast, which could be used for the determination of propranolol in plasma and pharmacokinetic studies.
