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高效液相色谱法测定1-三甲基硅基-1-炔-3-癸醇对映体纯度

Determination of Enantiomeric Purity of 1-Trimethylsilyl-1-decyn-3-ol by Chiral HPLC
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摘要 以苯甲酰氯试剂衍生1-三甲基硅基-1-炔-3-癸醇,得到具有强紫外吸收的1-三甲基硅基-1-癸炔-3-苯甲酸酯.考察流动相中不同醇调节剂、乙醇含量和柱温对外消旋1-三甲基硅基-1-癸炔-3-苯甲酸酯对映体在Chiralcel OD-H手性柱上色谱分离的影响,建立测定1-三甲基硅基-1-炔-3-癸醇对映体纯度的色谱分析方法.结果表明:以正己烷-乙醇(99.950.05,体积比)为流动相,检测波长为228nm,外消旋苯甲酰氯衍生对映体在Chiralcel OD-H柱上得到很好的分离,保留时间分别为6.94min和8.11min,分离因子和分辨率分别为1.41和3.75.本法灵敏度高,方法简便,适合于手性1-三甲基硅基-1-炔-3-癸醇样品的对映体纯度分析. A simple and accurate method for determination of the enantiomeric purity of 1-trimethylsilyl-1-decyn-3-ol by chiral hlgh-performance liquid chromatography was established. The 1-decyn-3-ol enantiomers were derivatized with benzoyl chloride by esterification to the benzoates,which could be detected sensitively by an UV monitor. The racemic 3-benzoyloxy -1-trimethylsilyl-l-decyne was completely resolved on Chiralcel OD-H column using n-hexane-ethanol （99.95 ： 0.05, by vol. ） as mobile phase in 9 minutes,the values of a and Rs were 1.41 and 3.75 respectively. The effects of different alcohol modifiers and ethanol percentage in mobile phase,as well as column temperature on chiral separation of the benzoate derivatives were discussed. Precision,linearity and limit of detection of the chromatographic method were also evaluated.
作者 阮源萍 孔俊琼 陈世礼 陈洁
机构地区 厦门大学化学化工学院 现代分析科学教育部重点实验室
出处 《厦门大学学报（自然科学版）》 CAS CSCD 北大核心 2008年第4期537-540,共4页 Journal of Xiamen University：Natural Science
基金 福建省自然科学基金(C0510001) 国家基础科学人才培养基金(J0630429)资助
关键词 高效液相色谱法 对映体拆分 1-三甲基硅基-1-炔-3-癸醇 紫外衍生 HPLC enantiomeric resolution 1-trimethylsilyl- 1-decyn-3-ol ultraviolet derivatization
分类号 O657.72 [理学—分析化学]
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厦门大学学报（自然科学版）
2008年 第4期

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