Abstract
The chiral synthesis of β-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.
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