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HPLC analysis method for (S)-2-aminopropanol

An aminopropanol and analysis method technology, applied in the field of high-performance liquid chromatography analysis of the chiral purity of -2-aminopropanol, can solve problems affecting levofloxacin, chiral isomers with weak ultraviolet absorption, etc., and facilitate standardized operation , stable properties and good reproducibility

Inactive Publication Date: 2018-02-09
SHANGHAI PUYI CHEM CO LTD
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  • Claims
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Problems solved by technology

The quality of (S)-2-aminopropanol, especially the chiral purity, directly affects the quality of levofloxacin. Therefore, the accuracy of the chiral detection method is very important. At present, there is no (S)-2- According to reports on the chiral detection of aminopropanol, (S)-2-aminopropanol and its chiral isomers have very weak UV absorption, so derivatization methods are usually used to enhance the UV absorption to improve detection sensitivity. Derivatization reagents and chromatographic conditions, enabling the detection to be completed in a short period of time is a basic problem that needs to be solved urgently

Method used

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  • HPLC analysis method for (S)-2-aminopropanol
  • HPLC analysis method for (S)-2-aminopropanol
  • HPLC analysis method for (S)-2-aminopropanol

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Embodiment 1

[0025] Embodiment 1: The chiral purity analysis of (RS)-2-aminopropanol

[0026] Precisely weigh about 25mg of (RS)-2-aminopropanol and put it in a 25ml measuring bottle, add about 0.2ml of derivatization reagent (derivatization reagent: 18g of tetrafluorobenzoic acid acetic anhydride, diluted with 200ml of anhydrous methanol), add mobile phase to dilute To the mark, shake well, take 0.5ml and add mobile phase to dilute to 10ml, as the test solution.

[0027] (1) Liquid chromatography condition A: ChromTech CHIRAL-AGP column, the mobile phase is 0.015mol / L phosphate aqueous solution-isopropanol (99:1), the UV detection wavelength is 320nm, the flow rate is 0.8 mL / min, the column The temperature was 30°C, and the injection volume was 20 μL. Retention time, resolution and chiral purity are shown in Table 1 below, and the spectrum is shown in figure 1 .

[0028] (2) Liquid chromatography condition B: ChromTech CHIRAL-AGP column, the mobile phase is 0.015 mol / L phosphate aqueou...

Embodiment 2

[0032] Embodiment 2: The chiral purity analysis of (S)-2-aminopropanol

[0033] Precisely weigh about 25 mg of (S)-2-aminopropanol and put it in a 25 ml measuring bottle, add about 0.2 ml of derivatization reagent (derivatization reagent: 18 g of tetrafluorobenzoic acid acetic anhydride, diluted with 200 ml of anhydrous methanol), add mobile phase to dilute To the mark, shake well, take 0.5ml and add mobile phase to dilute to 10ml, as the test solution.

[0034] (1) Liquid chromatography condition A: ChromTech CHIRAL-AGP column, the mobile phase is 0.015mol / L phosphate aqueous solution-isopropanol (99:1), the UV detection wavelength is 320nm, the flow rate is 0.8 mL / min, the column The temperature was 30°C, and the injection volume was 20 μL. Retention time, resolution and chiral purity are shown in Table 2 below, and the spectrum is shown in figure 2 .

[0035] (2) Liquid chromatography condition B: ChromTech CHIRAL-AGP column, the mobile phase is 0.015 mol / L phosphate aq...

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Abstract

The invention particularly relates to a method for detecting the chiral purity of (S)-2-aminopropanol. According to the present invention, 2,3,4,5-tetrafluorobenzoic acid acetic anhydride used as a derivatizing agent and (S)-2-aminopropanol are subjected to rapid derivatization in a methanol solvent at a room temperature to generate (S)-2,3,4,5-tetrafluoro-N-(1-hydroxy-2-yl)benzamide, and then detection analysis is performed by using HPLC-UV; and under the conditions of the method, the (S)-2-aminopropanol and the enantiomer derivative are effectively separated, the methodological results meetthe analysis determination requirements, and the method has advantages of rapidness, reliability, simple operation, good reproducibility and high sensitivity.

Description

technical field [0001] The invention belongs to the technical field of drug analysis, in particular to a high performance liquid chromatography analysis method for the chiral purity of (S)-2-aminopropanol. Background technique [0002] (S)-2-aminopropanol (III) is an important intermediate for the synthesis of levofloxacin. Levofloxacin is the S-type optical isomer of ofloxacin. Its antibacterial activity is twice that of the latter, and its toxicity and side effects are small. Water-soluble, in addition to oral dosage forms, it can also be made into injection dosage forms. The quality of (S)-2-aminopropanol, especially the chiral purity, directly affects the quality of levofloxacin. Therefore, the accuracy of the chiral detection method is very important. At present, there is no (S)-2- According to reports on the chiral detection of aminopropanol, (S)-2-aminopropanol and its chiral isomers have very weak UV absorption, so derivatization methods are usually used to enhance ...

Claims

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Application Information

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IPC IPC(8): G01N30/02
CPCG01N30/02
Inventor 王建忠
Owner SHANGHAI PUYI CHEM CO LTD
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