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Detection method of content of 1,5-dioxo-7ab-methyl-3aa-hexahydro indan-4a-propionic acid

A technology of hexahydroindene and methyl, which is applied in the detection field of pharmaceutical ingredients, achieves the effect of no solvent effect, wide application prospects, and less interference

Inactive Publication Date: 2017-07-14
SHANDONG SITO BIO TECHNOLOGY CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, since the compound does not have a chromophore and has no ultraviolet absorption, it cannot be detected by an ultraviolet absorption detector, so there is an urgent need for a method that can detect 1,5-dioxo-7ab-methyl-3aa-hexahydroindene Method for efficient separation and detection of full-4a-propionic acid

Method used

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  • Detection method of content of 1,5-dioxo-7ab-methyl-3aa-hexahydro indan-4a-propionic acid
  • Detection method of content of 1,5-dioxo-7ab-methyl-3aa-hexahydro indan-4a-propionic acid
  • Detection method of content of 1,5-dioxo-7ab-methyl-3aa-hexahydro indan-4a-propionic acid

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0056] (1) Weigh 25mg of the sample into a 50mL volumetric flask, and dissolve the sample with methanol as the solvent.

[0057] (2) After the sample solution described in step (1) is filtered through a 0.2 μm filter membrane, acetonitrile and water, acetonitrile and 0.2% formic acid aqueous solution are respectively used as mobile phases, and injected into a high performance liquid chromatograph for determination.

[0058] Instruments and reagents

[0059] Agilent 1260 HPLC.

[0060] Chromatographic column: ZORBAX SB-C18 250mm*4.6mm, 5μm.

[0061] The atomization temperature of the evaporative light scattering detector is 30-90° C., the temperature of the drift tube is 40-90° C., and the flow rate of the carrier gas is 1.0-1.8 bar.

[0062] Reagents: acetonitrile (chromatographically pure), distilled water (UP), formic acid, acetic acid or propionic acid (analytical pure).

[0063] Mobile phase ratio: V 乙腈 :V 水 =40:60V 乙腈 :V 0.2％甲酸水溶液 = 40:60.

[0064] Mobile phase fl...

Embodiment 2

[0070] (1) Accurately weigh the standard 1,5-dioxo-7ab-methyl-3aa-hexahydroindan-4a-propionic acid in a 50ml volumetric flask, dissolve it with methanol and dilute to the mark to prepare 0.6~0.7mg / ml sample solution, and serially diluted to obtain a series of sample concentrations of 0.4858, 0.3643, 0.2429, 0.1214 and 0.0607mg / ml.

[0071] (2) After the sample solutions of various concentrations prepared in step (1) are filtered through a 0.2 μm filter membrane, they are injected into a high-performance liquid chromatograph for measurement and the chromatograms corresponding to the sample solutions of various concentrations are drawn to further determine the sample solutions of each concentration For the corresponding peak area, take the concentration of the sample solution as the abscissa and the corresponding peak area as the ordinate, and draw the corresponding standard curve.

[0072] (3) Accurately weigh 21.68 mg of the sample to be tested in a 50 mL volumetric flask, di...

Embodiment 3

[0084] (1) Weigh 30mg of the sample into a 50mL volumetric flask, and dissolve the sample with methanol as the solvent.

[0085] (2) After the sample solution described in step (1) is filtered through a 0.2 μm filter membrane, acetonitrile and 0.1% acetic acid aqueous solution are used as mobile phases, and injected into a high-performance liquid chromatograph for determination.

[0086] Instruments and reagents

[0087] Agilent 1260 HPLC.

[0088] Chromatographic column: ZORBAX SB-C18 250mm*4.6mm, 5μm.

[0089] The atomization temperature of the evaporative light scattering detector is 30-90° C., the temperature of the drift tube is 40-90° C., and the flow rate of the carrier gas is 1.0-1.8 bar.

[0090] Reagents: acetonitrile (chromatographically pure), distilled water (UP), 0.1% acetic acid aqueous solution.

[0091] Mobile phase ratio: V 乙腈 :V 0.1％乙酸水溶液 =30:70.

[0092] Mobile phase flow rate: 1.0ml / min.

[0093] Sample injection volume: 20 μL.

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Abstract

The invention provides a detection method of the content of 1,5-dioxo-7ab-methyl-3aa-hexahydro indan-4a-propionic acid. As an evaporative light scattering detector (ELSD) is used, dioxo-7ab-methyl-3aa-hexahydro indan-4a-propionic acid without ultraviolet absorption can be detected. By means of the method provided by the embodiment of the invention, sample detection without ultraviolet band absorption can be realized. The method, as a universal analytic detection method, has a wide application prospect. According to the embodiment of the invention, the acid-base property of a moving phase is adjusted by an organic acid aqueous solution, so that the quantitative analysis and detection of 1,5-dioxo-7ab-methyl-3aa-hexahydro indan-4a-propionic acid are simply and quickly realized. According to the embodiment of the invention, as the ELSD is used to detect a sample, the method has the characteristics of being free of solvent effect, little in interference and the like, and meanwhile, the solvent is wide in compatibility.

Description

technical field [0001] The invention relates to the detection of pharmaceutical ingredients, in particular to a detection method for the content of 1,5-dioxo-7ab-methyl-3aa-hexahydroindan-4a-propionic acid. Background technique [0002] High-performance liquid chromatography is currently the most widely used chromatographic analysis method. The high-performance liquid chromatography system consists of a mobile phase liquid storage bottle, an infusion pump, a sampler, a chromatographic column, a detector and a recorder. The commonly used detector is an ultraviolet absorption detector, which is designed based on the principle that solute molecules absorb ultraviolet light. However, for some compounds without chromophore, due to no UV absorption, it is impossible to use UV absorption detectors for substance detection. [0003] 1,5-Dioxy-7ab-methyl-3aa-hexahydroindan-4a-propionic acid is a white powdery solid with the following structural formula: [0004] [0005] Its mole...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N30/02G01N30/06
CPCG01N30/02G01N30/06G01N2030/042
Inventor 刘芳马崇琳仝令华
Owner SHANDONG SITO BIO TECHNOLOGY CO LTD
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