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作 者:周琼[1] 石剑[2] 王桂平[1] 钱芳[1] 张彥焘 夏笔军[2]
机构地区:[1]广州医科大学卫生职业技术学院,广州510180 [2]南方医科大学药学院
出 处:《山东医药》2014年第36期4-7,共4页Shandong Medical Journal
基 金:国家自然科学基金资助项目(81102506/H3110);广州医学院青年科学基金资助项目(2010A02)
摘 要:目的:考察超高效液相色谱( UPLC)分析条件变化对汉黄芩苷转化因子( K)测定的影响。方法配制含汉黄芩苷、汉黄芩素(摩尔浓度比为1∶1)一系列浓度的标准溶液,经UPLC定量测得两化合物峰面积,二者比值即K值。逐个改变分析条件研究K值变化情况。结果随流动相pH值由2.5逐渐增至3.5、4.5、6.5,测得K值升高10.7%~14.6%;pH值增至8.5时两化合物出峰时间明显前移,影响分析准确性。随流动相离子强度、样品介质pH值变化,K值变化很小(偏差<4%)。检测波长由280 nm变至254、274、342 nm时,K值随之变化(4.1%~10.7%)。结论汉黄芩苷K值测定易受某些UPLC分析条件如流动相pH值、检测波长等变化的影响。对无对照品UGT代谢产物进行定量分析时,为保证结果准确可靠,在各种样品检测过程中最好保持分析条件完全一致。Objective To investigate the effects of UPLC analysis conditions on the conversion factor ( K) determina-tion of wogonoside .Methods A series of standard working solutions containing wogonoside and wogonin ( molar ratio 1∶1 ) were prepared and determined by UPLC to obtain peak area ratio of the two compounds , which was equal to the value of K.Then, analysis conditions were altered respectively and observed the variance of K value .Results When pH value of mobile phase A rose from 2.5 to 3.5, 4.5 and 6.5, K values were found to increase 10.7%-14.6%.When the pH value rose to 8.5, the retention time of wogonoside and wogonin moved forward significantly , which affected the accuracy of K value determination .With the variance of ionic strength of mobile phase A and pH value of sample medium , the K values determined were similar (deviation〈4%).With the variance of detection wavelength from predetermined 280 nm to 254, 274, 342 nm, deviation of K value was in the range of 4.1%-10.7%.Conclusions The K value determination of wogonoside is susceptible to the variance of several UPLC analysis conditions such as pH value of mobile phase A , detection wavelength .To provide more precise quanification for glucuronides which are usually not available commercially , it is nec-essary to keep UPLC analysis conditions consistent during the process of determination .
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