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红豆杉属植物中10 - 去乙酰巴卡亭III及相关紫杉烷类化合物的固相萃取与简化高效液相色谱测定

Solid-phase extraction and simplified high-performance liquid chromatographic determination of 10-deacetylbaccatin III and related taxoids in yew species.

作者信息

Mroczek T, Glowniak K

机构信息

Department of Pharmacognosy, Medical University, Peowiakow 12 St., 20007 Lublin, Poland.

出版信息

J Pharm Biomed Anal. 2001 Aug;26(1):89-102. doi: 10.1016/s0731-7085(01)00353-3.

Abstract

Solid-phase extraction was accomplished with specially prepared cartridges filled with silanised silica gel (RP-2) for the purpose of 10-deacetylbaccatin III (10-DAB III) and related taxoids extracts purification obtained from different yew materials. In the first method, the analysed taxoids eluted in 75% methanol, but in the second method, the preliminary elution with 30% methanol was made. DAB III and its six derivatives were separated from co-extractives in merely acetonitrile-water gradient mode during 25 min on Waters Symmetry C-18 column with photodiode array (PDA) detection. The total recoveries for 10-DAB III and paclitaxel in the first SPE method (all compounds were applied in amounts of 80 microg) were about 98 and 94%, respectively. Almost 100% recoveries for paclitaxel and baseline separation of 10-DAB III and co-extracted compounds were obtained when preliminary elution with 30% methanol was performed. This method can be applied as a routine, inexpensive and uncomplicated procedure for 10-DAB III and related taxoids determination in yew material.

摘要

采用装有硅烷化硅胶(RP - 2)的特制柱进行固相萃取,目的是纯化从不同紫杉材料中获得的10 - 去乙酰巴卡亭III(10 - DAB III)及相关紫杉烷类提取物。在第一种方法中,分析的紫杉烷类化合物用75%甲醇洗脱,但在第二种方法中,先用30%甲醇进行初步洗脱。在Waters Symmetry C - 18柱上,通过光电二极管阵列(PDA)检测,在25分钟内仅以乙腈 - 水梯度模式从共提取物中分离出DAB III及其六种衍生物。在第一种固相萃取方法中(所有化合物的应用量均为80微克),10 - DAB III和紫杉醇的总回收率分别约为98%和94%。当用30%甲醇进行初步洗脱时,紫杉醇的回收率几乎达到100%,并且10 - DAB III与共提取化合物实现了基线分离。该方法可作为一种常规、廉价且简单的程序,用于测定紫杉材料中的10 - DAB III及相关紫杉烷类化合物。

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