十二烷基键合固定相的制备及在青霉素降解研究中的应用

Preparation of a Dodecyl Bonded Stationary Phase and Its Application in Separation of Degradation Products of Penicillin

采用 2 ,4 -戊二酮与正十二烷基二甲基氯硅烷在咪唑的催化下制成活泼的中间体——硅醚烷基中间体 ,再与硅胶进行键合 ,用元素分析法测得该固定相中 C的质量分数为 9.6 8%。利用该固定相 ,在流动相为乙腈 -0 .0 2 m ol/L磷酸盐缓冲液 (p H 6 .0 ) (30∶ 70 ,含 0 .0 0 6 mol/L氯化四丁基铵 )的条件下成功地分离了青霉素 G及其三种主要降解产物。

The alkyl silyl enol ethers of pentane-2,4-dione, prepared from alkylchlorosilane and pentane-2,4-dione in the presence of imidazole, was bonded with silica gel to obtain the stationary phase with carbon content of 9.68%. Penicillin G and its three major degradation products could be separated by using this stationary phase with the mobile phase of acetonitrile-0.02mol/L phosphate buffer solution(pH6.0)(30∶70, containing 0.006mol/L tetrabutylammonium chloride).