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The enantiomericpuritydeterminationofasyntheticintermediateofnew3,4-dihydro-2,2-dimethyl-2H- 1-benzopyrans, i.e.4-amino-2,2-dimethyl-6-ethoxycarbonylamino-3,4-dihydro-2H-1-benzopyran, was successfully carriedoutusingananioniccyclodextrin(CD)derivativecombinedwithachiralionic liquid (IL).Inordertoobtainhighresolutionandefficiencyvalues,theadditionofachiralIL,i.e. ethylcholine bis(trifluoromethylsulfonyl)imide(EtCholNTf2), tothebackgroundelectrolytecontain- ing heptakis(2,3-di-O-methyl-6-O-sulfo)--CD (HDMS--CD) wasfoundtobeessential.Asimultaneous increase inseparationselectivityandenantioresolutionseemstoindicateasynergisticeffectofHDMS-- CD andEtCholNTf2. Thebestenantioseparationofthekeyintermediatewasachievedusingamethanolic solution of0.75Mformicacid,10mMammoniumformate,1.5mMHDMS--CD and5mMEtCholNTf2. Levamisole wasselectedasinternalstandard.Theoptimizedconditionsallowedthedeterminationof 0.1% ofeachenantiomerinthepresenceofitsstereoisomerusingthemethodofstandardadditions.The NACE methodwasthenfullyvalidatedwithrespecttoselectivity,responsefunction,trueness,precision,accuracy, linearityandlimitsofdetectionandquantification. |
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2Â¥2010-09-16 19:28:02
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3Â¥2010-09-16 20:28:29
Æ»¹ûÁ³_2009
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4Â¥2010-09-16 23:22:46
xjyuefan
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5Â¥2010-09-17 00:15:47
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The enantiomeric purity determination of a synthetic intermediate of new 3,4-dihydro-2,2-dimethyl-2H- 1-benzopyrans, i.e.4-amino-2,2-dimethyl-6-ethoxycarbonylamino-3,4-dihydro-2H-1-benzopyran, was successfully carried out using an anionic cyclodextrin(CD) derivative combined with a chiral ionic liquid (IL).In order to obtain high resolution an defficiency values,the addition of a chiralIL,i.e. ethylcholine bis(trifluoromethylsulfonyl)imide(EtCholNTf2), to the background electrolytecontain- ing heptakis(2,3-di-O-methyl-6-O-sulfo)--CD (HDMS--CD) was found to be essential.A simultaneous increase in separation selectivity andenantioresolution seems to indicate asynergistic effect of HDMS-- CD and EtCholNTf2. The best enantioseparation of the key intermediate was achieved using a methanolic solution of0.75M formic acid,10mM ammonium formate,1.5mMHDMS--CD and 5mM EtCholNTf2. Levamisole was selected as internal standard.The optimized conditions allowed the determination of 0.1% of each enantiomer in the presence of its stereoisomer using the method of standard additions.The NACE method was then fully validated with respect to selectivity,response function,trueness,precision,accuracy, linearity and limits of detection and quantification. |

7Â¥2010-09-17 08:19:06
jiangmingj
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8Â¥2010-09-17 08:34:31
lfycdymax
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9Â¥2010-09-17 09:15:50









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