A method for separating r/s-3-quinuclidinol by pre-column derivatization high performance liquid chromatography

Abstract

The invention discloses a method for resolving R / S-3-quinuclidinol by pre-column derivatization high-performance liquid chromatography, that is, firstly, R / S-3-quinuclidinol is obtained through pre-column derivatization esterification reaction R / S-3-quinuclidinol ester, then use high-performance liquid chromatography, using amylose chiral column as chromatographic column, using a mixture of n-hexane, alcohol and alkaline additives as the normal phase mobile phase , the above-mentioned R / S-3-quinuclidinol ester was made into a sample solution with a concentration of 1.0 mg / mL, the flow rate was controlled to be 0.6-1 mL / min, the injection volume was 5 μL, and the detection wavelength was 220-280 nm. The column temperature is 20-35°C, and the above-obtained R / S-3-quinuclidinyl ester is subjected to chiral separation. The chromatographic peak shape and symmetry obtained by the separation method are better, and the separation degree is higher, and the R / S-3-quinuclidinol ester can be effectively, rapidly and sensitively detected and resolved.

Description

technical field [0001] The invention relates to a method for separating R / S-3-quinuclidinol by pre-column derivatization high-performance liquid chromatography, that is, derivatizing R / S-3-quinuclidinol before the column to obtain derivatives with ultraviolet absorption , and then the derivatives were separated and detected by chiral chromatographic column and ultraviolet detector. Background technique [0002] The chemical name of R-3-quinuclidin is 1-azacyclo-[2,2,2]-octyl-R-3-ol, which is used to study human erythrocyte acetylcholinesterase and synthesize several muscarinic receptors It is an important intermediate of body antagonist drugs such as solifenacin, ravatorate, tasalidine, etc. It is also the precursor of chiral liquid catalysts and is widely used in chiral catalysis. At present, most drugs are mainly administered as racemates, and the administration of optically pure enantiomers is the development trend of most chiral drugs. Therefore, the research on the c...

AI Technical Summary

Problems solved by technology

[0005] The object of the present invention is to provide a kind of utilizing pre-column derivatization high-performance liquid chromatography to resolve R / S- The method of 3-quinuclidinol, which can overcome the defects and deficiencies of the existing analytical methods, makes the operation simple and convenient, rapid and sensitive detection, good chromatographic peak shape and symmetry, high resolution, and more effective detection and split R / S-3-quinuclidinol

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