Determination of the enantiomers of 3-tert.-butylamino-1,2-propanediol by high-performance liquid chromatography using mass spectrometric detection.
The chiral synthesis of beta-blockers such as (S)-timolol requires a sensitive analytical method for the enantioseparation of its intermediate, 3-tert.-butylamino-1,2-propanediol, in the ng/ml range. The method developed is based on on-line normal-phase LC-MS-MS using a chiral stationary phase and an atmospheric pressure chemical ionization (APCI) interface. The MS detection of 3-tert.-butylamino-1,2-propanediol was first optimized with a pneumatically-assisted electrospray interface (ionspray). The APCI interface was then selected for LC-MS-MS because of the incompatibility of electrospray with n-hexane. The method was validated for both enantiomers in the 25-500 ng/ml concentration range.
Toussaint
B
B
Department of Analytical Pharmaceutical Chemistry, Institute of Pharmacy, University of Liège, CHU, Belgium. b.toussaint@ulg.ac.be
Streel
B
B
Ceccato
A
A
Hubert
P
P
Crommen
J
J
D001274:Atmospheric Pressure; D002851:Chromatography, High Pressure Liquid / Q000379:methods*; D013058:Mass Spectrometry; D011409:Propylene Glycols / Q000032:analysis*; D015203:Reproducibility of Results; D012680:Sensitivity and Specificity; D013237:Stereoisomerism
C418769:3-tert-butylamino-1,2-propanediol; D011409:Propylene Glycols