柱前衍生化高效液相色谱法测定乳酸的光学纯度  被引量:5

Determination of enantiomeric purity of lactic acid by pre-column derivatization-high performance liquid chromatography

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作  者:杨丹[1] 徐旭[1] 陈宇静[1] 张林[1] 姚长洪[1] 宋航[1] 

机构地区:[1]四川大学制药与生物工程系,成都610065

出  处:《分析试验室》2008年第4期52-55,共4页Chinese Journal of Analysis Laboratory

基  金:四川大学星火计划项目资助

摘  要:用苯胺将乳酸衍生化,得到的对映体衍生物在DNB-Leucine柱上进行了拆分,建立了一种用柱前手性衍生化结合手性固定相正相高效液相色谱法检测乳酸光学纯度的方法,并考察了流动相组成和柱温对其分离的影响。分离结果经二极管阵列紫外检测器检测,以及与对照品比较得到确认。当流动相为V(正己烷)∶V(乙醇)=90∶10,温度为25℃,流速为1.5 mL/min时,乳酸达到基线分离,分离因子达1.30以上。将此法测定乳酸光学纯度的结果与旋光仪方法测定的结果进行比较,相对偏差不超过2%。本方法可用于乳酸对映体的光学纯度准确检测。Lactic acid was derivatized with aniline,and then the enantiomers of the derivatives were separated on the DNB-Leucine column.A new method for accurately measuring enantiomeric purity of lactic acid was established by derivatization combined with CSP.The influences of mobile phase composition and column temperature on separation were investigated.The separating result was confirmed by the diode array ultraviolet detector and compared with the reference substance.When the mobile phase composition was 90% hexane and 10% ethanol(volume) at a flow rate of 1.5 mL/min at 25 ℃,lactic acid was separated on the baseline and the separation factor was more than 1.30.Compared with the result of enantiomeric purity of lactic acid determined by polarimeter,the relative deviation is less than 2%.This method is simple,sensitive with good repeatability,and can be used to measure the enantiomeric purity of lactic acid accurately.

关 键 词:高效液相色谱 衍生化 手性拆分 光学纯度 乳酸 

分 类 号:O657.7[理学—分析化学]

 

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