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目的建立一种快速高效的盐酸昂丹司琼对映体分离方法,检查盐酸左昂丹司琼(R型)中异构体含量。方法手性柱为CHIRALPAK IC(4.6 mm×250 mm,5μm);流动相:正己烷-无水乙醇-乙二胺(50∶50∶0.1);检测波长:245 nm;流速:1.0 m L·min-1;柱温:25℃。同时考察了醇改性剂的种类、比例、有机添加剂二乙胺的比例、流速、温度等因素对拆分的影响。结果盐酸昂丹司琼对映体在CHIRALPAK IC手性柱上分离度为6.5,盐酸左昂丹司琼中含0.02%的右旋异构体可被检出。结论方法专属性好、灵敏度高,适用于盐酸昂丹司琼对映体的分离以及盐酸左昂丹司琼中右旋异构体杂质的测定。
OBJECTIVE To establish a rapid and efficient method for the separation of ondansetron hydrochloride enantiomers and to determine the content of isomers in lev- dodexan hydrochloride (R type). METHODS The chiral column was CHIRALPAK IC (4.6 mm × 250 mm, 5 μm). The mobile phase consisted of n-hexane - absolute ethanol - ethylenediamine (50:50:0.1). The detection wavelength was 245 nm. min-1; column temperature: 25 ℃. At the same time, the effects of factors such as the type and proportion of alcohol modifier, the proportion of diethylamine added by organic additives, flow rate and temperature on the resolution were investigated. Results The ondansetron hydrochloride enantiomer showed a resolution of 6.5 on a CHIRALPAK IC chiral column and a 0.02% dextrorotatory isomer in levonistan hydrochloride. Conclusion The method has good specificity and high sensitivity. It is suitable for the separation of ondansetron hydrochloride enantiomers and dextroisomer hydrochloride dextroisomer impurity determination.