Mroczek T, Glowniak K
Department of Pharmacognosy, Medical University, Peowiakow 12 St., 20007 Lublin, Poland.
J Pharm Biomed Anal. 2001 Aug;26(1):89-102. doi: 10.1016/s0731-7085(01)00353-3.
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.
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。
