超临界流体色谱法分离碱性药物

众所周知，具有高极性材料柱的SFC显示出与正相色谱相同的保留作用，因此被认为难以分离含水的高极性组分。然而，如果在改性剂溶剂（醇等）中加入少量挥发性酸、碱或盐，则可以改善极性组分峰的形状，并且可以用适当的保留时间洗脱保留时间长的组分。以甲醇中的乙酸铵为改性溶剂，采用2-乙基吡啶柱对各种碱性药物进行了分离。Application Note 2/2Application NoteSeparation of Basic Drugs by Supercritical Fluid Chromatography Separation of Basic Drugs by Supercritical Fluid Chromatography In t rod u c t ion It is well kn o wn t hat SFC with a column of high polarity mater i al shows the same retention action as normal phase chromatography ， and t herefore it is bel i eved to be difficult to separate aqueous high polar i ty compo n ents. However， if a li tt le vo l atile acid， base ， or sal t is added to m odifier solvent (alcohol or etc.)， the shape of polar component ’s peak can be improved， and components with a long retention t i me can be eluted with an appropri a te retent i on ti me. Various basic drugs were separated using the 2-Ethylpyridine column with ammonium acetate in methan o l as modi f ier solvent . Keywords： SFC， Basic Drugs， achira l ， 2-Ethylpyridine column， PDA Detector CO2 Del i very PU-2080-CO2Column：2-Ethylpyridine 60A (4.6 mmID P um p：x 250 mmL ， 5 pm) (Prin c eton Modifier Pump：PU-2080Chromatography Inc .)MCixer：MX-2080-32O2 Flow rate：3.0mL/min Autosampler ：AS-2059-SF Modifier：20 mM Ammonium acetate inM Cethanololumn Oven：CO-2060PDA Detector：MD-2018Modif i er gradient ：0 mi n (0.2 mL /mi n )， 6 m in (0.2 mL/[H igh pressure cell]m i n)， 13 min (1.0 mL/min)， 18 mi n Back Pressure BP-2080(1.0 mL /mi n )， 18.05 m i n (0.2mL /min)，Regulator：1 cycle： 30 min Column temp.：40°C Back Pressure：15 MPa Wavelength：200-400nm I njection volume：5uL Sta n dard sample：Mixture 0.1 mg/mL each Results C h r o m a t o gr a m a n d c o nt o u r p l o t o f s t an d ard mix tu r e o f b a s i c dru g s (220n m ) ar e sh o wn i n f igu re 1.As s h own ， pola r comp o n e n ts su ch a s B e r be r i n e a nd M a l e i c w e r e a l s o el u t e d . Fi g ure 1. Chroma t ogram of st a ndard m i xt u re of b as ic dru g s1： Ca ffe i n e ， 2： Hexo b a r b i ta l ， 3：Amitrip t yli n e， 4：Ch l orp h e n irami n e， 5： I mipra m ine 6： Q u i n i n e， 7：A t ro p i n e， 8：Acetamin o p hen ， 9：Berberin e ， 10： Male i c acid