Kim K H, Kim H J, Hong S P, Shin S D
College of Pharmacy, Kangwon National University, Chunchon, Korea.
Arch Pharm Res. 2000 Oct;23(5):441-5. doi: 10.1007/BF02976568.
Achiral-chiral column switching HPLC assay was developed to allow the separation and quantification of the enantiomers of terbutaline in human plasma by means of fluorescence detection. Plasma samples were prepared by solid-phase extraction with sep-pak silica, followed by HPLC assay. The enantiomers of terbutaline and the internal standard were separated from the biological matrix on a silica column, and the two enantiomers were resolved and quantified on a Sumichiral OA-4900 column. The two columns were connected by a switching valve equipped with silica trap column. The trap column was used to concentrate the terbutaline in the eluent from the achiral column before back flushing onto the chiral phase. For each enantiomers, the assay was linear between 2.5-125 ng/ml (r=0.9999) and detection limit was 1.0 ng/ml.
建立了非手性-手性柱切换高效液相色谱法,通过荧光检测对人血浆中的特布他林对映体进行分离和定量。血浆样品采用硅胶固相萃取法制备,然后进行高效液相色谱分析。特布他林对映体和内标物在硅胶柱上与生物基质分离,两种对映体在Sumichiral OA - 4900柱上进行分离和定量。两根柱子通过配备硅胶捕集柱的切换阀连接。捕集柱用于在将非手性柱流出物反冲到手性相之前浓缩其中的特布他林。对于每种对映体,该分析方法在2.5 - 125 ng/ml之间呈线性(r = 0.9999),检测限为1.0 ng/ml。