山东医药
山東醫藥
산동의약
SHANDONG MEDICAL JOURNAL
2014年
36期
4-7
,共4页
周琼%石剑%王桂平%钱芳%张彥焘%夏笔军
週瓊%石劍%王桂平%錢芳%張彥燾%夏筆軍
주경%석검%왕계평%전방%장언도%하필군
转化因子%UPLC分析条件%汉黄芩苷%汉黄芩素
轉化因子%UPLC分析條件%漢黃芩苷%漢黃芩素
전화인자%UPLC분석조건%한황금감%한황금소
conversion factor%UPLC analysis conditions%wogonoside%wogonin
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。
目的:攷察超高效液相色譜( UPLC)分析條件變化對漢黃芩苷轉化因子( K)測定的影響。方法配製含漢黃芩苷、漢黃芩素(摩爾濃度比為1∶1)一繫列濃度的標準溶液,經UPLC定量測得兩化閤物峰麵積,二者比值即K值。逐箇改變分析條件研究K值變化情況。結果隨流動相pH值由2.5逐漸增至3.5、4.5、6.5,測得K值升高10.7%~14.6%;pH值增至8.5時兩化閤物齣峰時間明顯前移,影響分析準確性。隨流動相離子彊度、樣品介質pH值變化,K值變化很小(偏差<4%)。檢測波長由280 nm變至254、274、342 nm時,K值隨之變化(4.1%~10.7%)。結論漢黃芩苷K值測定易受某些UPLC分析條件如流動相pH值、檢測波長等變化的影響。對無對照品UGT代謝產物進行定量分析時,為保證結果準確可靠,在各種樣品檢測過程中最好保持分析條件完全一緻。
목적:고찰초고효액상색보( UPLC)분석조건변화대한황금감전화인자( K)측정적영향。방법배제함한황금감、한황금소(마이농도비위1∶1)일계렬농도적표준용액,경UPLC정량측득량화합물봉면적,이자비치즉K치。축개개변분석조건연구K치변화정황。결과수류동상pH치유2.5축점증지3.5、4.5、6.5,측득K치승고10.7%~14.6%;pH치증지8.5시량화합물출봉시간명현전이,영향분석준학성。수류동상리자강도、양품개질pH치변화,K치변화흔소(편차<4%)。검측파장유280 nm변지254、274、342 nm시,K치수지변화(4.1%~10.7%)。결론한황금감K치측정역수모사UPLC분석조건여류동상pH치、검측파장등변화적영향。대무대조품UGT대사산물진행정량분석시,위보증결과준학가고,재각충양품검측과정중최호보지분석조건완전일치。
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 .