生物转化体系中R-肾上腺素光学纯度的测定  被引量:3

Determination of the Optical Purity of Biotransfortated R-adrenaline

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作  者:林美新[1] 陈必钦[1] 李忠琴[2] 许小平[1] 

机构地区:[1]福州大学化学化工学院,福建福州350002 [2]集美大学水产学院,福建厦门361021

出  处:《分析科学学报》2010年第4期395-399,共5页Journal of Analytical Science

基  金:福建省自然科学基金(No.2008J0100);福建省科技计划重点项目(No.2009N0046);集美大学博士科研启动基金(No.ZQ2008015);集美大学优秀青年骨干教师基金(No.2008C001)

摘  要:以羟丙基-β-环糊精(HP-β-CD)为手性选择剂,采用高效毛细管电泳技术,对肾上腺素对映体拆分进行了研究。以55mmol/LTris-磷酸(含30g/LHP-β-CD,pH2.5)为运行缓冲液,分离电压23kV,柱温22℃,采用压力正极进样(3kPa×4s),肾上腺素对映体于13min内获得良好分离(RS=2.12)。在波长214nm处进行紫外检测,迁移时间和峰面积的相对标准偏差≤3.7%,峰面积与S-肾上腺素含量在0.3~130μg/L范围内呈良好的线性关系(相关系数为0.9951),回收率在97.5%~102.5%之间,肾上腺素对映体检出限(S/N=3)可达0.1μg/L,将其应用于手性生物转化样品分析,可很好地检测出R-肾上腺素的光学纯度。本研究为该类药物的生物不对称转化提供了很好的分析方法。The enantiomeric separation of adrenaline was obtained by high performance capillary electrophoresis using hydroxypropyl-β-cyclodextrin(HP-β-CD) as the chiral selector. 55 mmol/L Tris-H3PO4 buffer at pH=2.5 containing 30 g/L HP-β-CD was chosen as the running electrolyte. The separation was performed at 22℃ with a positive voltage of 23 kV. Samples were injected into well within 13 min(RS=2.12). Coupled with ultraviolet detection,an excellent linear range from 0.3 to 130 μg/L (r=0.9951) for the detemination of adrenaline enantiomers was exhibited. The RSD for migration time and peak area were both lower than 3.7%. The recovery was 97.%~102.5%,and the detection limit (S/N=3) was 0.1 μg/L. The enantiomeric separation method has been applied for the determination of fermentation broth samples. It may be used as a good method for the quality control of adrenergic drugs.

关 键 词:毛细管电泳法 R-肾上腺素 对映体分离 光学纯度检测 

分 类 号:O657.8[理学—分析化学]

 

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