کد مقاله کد نشریه سال انتشار مقاله انگلیسی نسخه تمام متن
1199182 1493563 2014 13 صفحه PDF دانلود رایگان
عنوان انگلیسی مقاله ISI
Enantioseparation of pyroglutamide derivatives on polysaccharide based chiral stationary phases by high-performance liquid chromatography and supercritical fluid chromatography: A comparative study
ترجمه فارسی عنوان
انعطاف پذیری مشتقات پریو گلوتامید در فازهای ثابت کریال مبتنی بر پلی ساکارید با استفاده از کروماتوگرافی مایع با کارایی بالا و کروماتوگرافی مایع سوپر کریتیک: یک مطالعه مقایسه ای
موضوعات مرتبط
مهندسی و علوم پایه شیمی شیمی آنالیزی یا شیمی تجزیه
چکیده انگلیسی


• Pyroglutamide derivatives known as h-P2X7 receptor antagonists.
• Enantioseparation on polysaccharide based chiral stationary phases.
• Comparative study of preparative HPLC and SFC.
• Validation of the determination of the enantiomeric purity.

Analytical enantioseparation of three pyroglutamide derivatives with pharmacological activity against the purinergic receptor P2X7, was run in both high-performance liquid chromatography and supercritical fluid chromatography. Four polysaccharide based chiral stationary phases, namely amylose and cellulose tris (3,5-dimethylphenylcarbamate), amylose tris ((S)-α-methylbenzylcarbamate) and cellulose tris (4-methylbenzoate) with various mobile phases consisted of either heptane/alcohol (ethanol and 2-propanol) or carbon dioxide/alcohol (methanol or ethanol) mixtures, were investigated. After analytical screenings, the best conditions were transposed, for compound 1, to semi-preparative scale. Each approach was fully validated to meet the International Conference on Harmonisation requirements and compared. Whereas the limits of detection and quantification were near six-fold better in HPLC than in SFC (respectively 0.20 and 0.66 μM versus 1.11 and 3.53 μM for one of the enantiomers), in terms of low solvent consumption (7.2 mL of EtOH versus 3.2 mL of EtOH plus 28.8 mL of toxic and inflammable heptane per injection in SFC and HPLC, respectively), time effective cost (9 min versus 40 min per injection in SFC and HPLC, respectively) and yields (98% versus 71% in SFC and HPLC, respectively), the latter method proved its ecological superiority.

ناشر
Database: Elsevier - ScienceDirect (ساینس دایرکت)
Journal: Journal of Chromatography A - Volume 1363, 10 October 2014, Pages 257–269
نویسندگان
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