介绍了一种检测肉碱和酰基肉碱的策略。该通用系统具有四个组成部分:(1)通过蛋白质沉淀/脱盐和阳离子交换固相萃取进行分离,(2)肉碱和酰基肉碱用五氟苯甲酰基三氟甲磺酸酯的衍生化,(3)顺序离子交换/反相色谱,使用单个未封端的C8色谱柱,以及(4)使用离子阱质谱仪检测肉碱和酰基肉碱五氟苯甲酸酯。从分离过程中回收的肉碱和酰基肉碱为77-85%。衍生化迅速且完全,没有酰基肉碱水解的迹象。顺序离子交换/反相HPLC可分离衍生自肉碱和酰基肉碱的试剂副产物,然后反相分离肉碱和酰基肉碱五氟苯甲酸酯。MS / MS的检测具有高度选择性,其中肉碱五氟苯甲酸酯在m / z 311处产生强的产物离子,酰基肉碱五氟苯甲酸酯碎片产生两个产物离子:(1)m / z 59的损失和(2)离子的产生在m / z 293上进行分析。为证明该分析策略,将磷酸缓冲的血清白蛋白掺入了肉碱和15种酰基肉碱,并使用上述蛋白沉淀/脱盐和阳
作者:A. L. Fridman、É. G. Yufareva、Yu. A. Kozhevnikov、V. S. Zalesov、N. A. Kolobov
DOI:10.1007/bf00758355
日期:1976.2
We have studied the reac t ion of N-carboxymethylsydnone with some aliphaticdiazocompounds. For this purpose we used diazomethane, phenyldiazomethane, diphenyldiazomethane, diazofluorene, ethyl d iazoace ta te , and a s e r i e s of a d i a z o ketches with different subst i tuents , viz . alkyl, adamantyl , and ary l . In all c a ses , we succeeded in isolat ing the cor responding N-carboxymethylsydnone
Five ketenes, phenyl(ethyl)ketene, phenyl(methylthio)ketene, diphenylketene, pentafluorophenylketene, and 1-naphthylketene, were generated flash photolytically and solvent isotope effects (H2O vs. D2O) on their hydroxide-ion-catalyzed hydration in aqueous solution were determined. The values obtained are all weakly inverse and closely similar (k(HO)/k(DO) = 0.76-0.97), as expected for these fast, hydroxide-ion-consuming reactions, known to proceed by nucleophilic attack of hydroxide on the ketene carbonyl group. The characteristic magnitude of these isotope effects should prove useful in identifying new examples of this reaction.
FRIDMAN A. L.; YUFAREVA EH. G.; KOZHEVNIKOV YU. A.; ZALESOV V. S.; KOLOBO+, XIM.-FARMATSEVT. ZH. <KNFZ-AN>, 1976, 10, HO 2, 53-56
作者:FRIDMAN A. L.、 YUFAREVA EH. G.、 KOZHEVNIKOV YU. A.、 ZALESOV V. S.、 KOLOBO+
DOI:——
日期:——
GEMINAL BISPHOSPHONIC ACIDS AND DERIVATIVES AS ANTI-ARTHRITIC AGENTS