Source:http://linkedlifedata.com/resource/pubmed/id/16445925
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rdf:type | |
lifeskim:mentions | |
pubmed:issue |
1-2
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pubmed:dateCreated |
2006-6-19
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pubmed:abstractText |
Mixtures of hexane-like ethoxynonafluorobutane with alcohols were used as MS-friendly mobile phases for separation and efficient detection of non-UV-active enantiomers and diastereomers using normal-phase HPLC-APCI-MS. Racemic muscone, camphorsulfonamide, camphorsultam, BOC-protected 1-(3-aminopropyl)-2-pipecoline and diastereomeric 2-methylhexanoyl camphorsultams were resolved on Chiralpak AS and AD and achiral Luna CN columns. The responses of UV and APCI-MS detectors were compared under separation conditions studied, with MS detection achieving lowest detectable quantity in the range of 0.5-2 ng per chromatographic peak. The absolute configuration of crystalline derivatives of racemic 2-methylhexanoic acid with (S)-(-)-2,10-camphorsultam was determined by X-ray analysis after their automatic purification by preparative LC-MS. The technique described can be used to purify and determine the absolute stereochemistry of compounds of unknown structure which contain free carboxy group and lack sufficient UV absorbance.
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pubmed:language |
eng
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pubmed:journal | |
pubmed:citationSubset |
IM
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pubmed:chemical |
http://linkedlifedata.com/resource/pubmed/chemical/Butanes,
http://linkedlifedata.com/resource/pubmed/chemical/Cycloparaffins,
http://linkedlifedata.com/resource/pubmed/chemical/Hydrocarbons, Fluorinated,
http://linkedlifedata.com/resource/pubmed/chemical/Pharmaceutical Preparations,
http://linkedlifedata.com/resource/pubmed/chemical/ethoxynonafluorobutane,
http://linkedlifedata.com/resource/pubmed/chemical/muscone
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pubmed:status |
MEDLINE
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pubmed:month |
Jul
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pubmed:issn |
0021-9673
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pubmed:author | |
pubmed:issnType |
Print
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pubmed:day |
7
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pubmed:volume |
1120
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pubmed:owner |
NLM
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pubmed:authorsComplete |
Y
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pubmed:pagination |
82-8
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pubmed:dateRevised |
2009-1-15
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pubmed:meshHeading |
pubmed-meshheading:16445925-Butanes,
pubmed-meshheading:16445925-Chromatography, High Pressure Liquid,
pubmed-meshheading:16445925-Cycloparaffins,
pubmed-meshheading:16445925-Hydrocarbons, Fluorinated,
pubmed-meshheading:16445925-Molecular Structure,
pubmed-meshheading:16445925-Pharmaceutical Preparations,
pubmed-meshheading:16445925-Reproducibility of Results,
pubmed-meshheading:16445925-Spectrometry, Mass, Electrospray Ionization,
pubmed-meshheading:16445925-Stereoisomerism,
pubmed-meshheading:16445925-Ultraviolet Rays
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pubmed:year |
2006
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pubmed:articleTitle |
Normal-phase chiral liquid chromatography-mass spectrometry of non-UV-active compounds: applications for pharmaceutically relevant racemates.
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pubmed:affiliation |
Discovery Analytical Chemistry, Chemical Sciences, Wyeth Research, CN 8000, Princeton, NJ 08540, USA. kaganm@wyeth.com
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pubmed:publicationType |
Journal Article
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