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Analysis method for determining related substances in glimepiride intermediate by utilizing HPLC (High Performance Liquid Chromatography)

An analytical method and technology for related substances are applied in the field of chemical drug analytical method development to achieve the effects of convenient operation, high sensitivity and stability, and efficient elution

Pending Publication Date: 2022-04-01
XUZHOU WANBANG JINQIAO PHARMA +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

There are no four known impurities in the chromatographic purity test and the calculation of the impurity correction factor

Method used

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  • Analysis method for determining related substances in glimepiride intermediate by utilizing HPLC (High Performance Liquid Chromatography)
  • Analysis method for determining related substances in glimepiride intermediate by utilizing HPLC (High Performance Liquid Chromatography)
  • Analysis method for determining related substances in glimepiride intermediate by utilizing HPLC (High Performance Liquid Chromatography)

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0048] Comparison of different chromatographic columns in Example 1

[0049] HPLC conditions:

[0050] Performed on Agilent Poroshell 120PFP column (150*4.6mm, 2.7μm), Welch UltimateAQ-C18 column (250*4.6mm, 5μm), Welch Ultimate XB-C18 column (250*4.6mm, 5μm) In the test, the volume ratio of 0.01mol / L ammonium dihydrogen phosphate buffer solution with a pH of 3.5 adjusted by phosphoric acid and methanol was 50:50 as the mobile phase, the detection wavelength was 225nm, and the flow rate was 1.0ml / min or 0.5ml / min. The column temperature was 25°C, the injection volume was 20 μl, and isocratic elution was performed.

[0051] Sample preparation:

[0052] System suitability solution: Weigh appropriate amount of benzenesulfonamide reference substance and each impurity reference substance to prepare each 1ml containing about 0.1 mg of benzenesulfonamide reference substance, 0.5 μg of impurity A, 0.5 μg of impurity B, 0.5 μg of impurity C and impurities. D 0.5μg mixed solution.

...

Embodiment 2

[0057] The contrast of embodiment 2 organic phase

[0058] HPLC conditions:

[0059] Methanol was used as the organic phase and acetonitrile was used as the organic phase. The chromatographic column was an Agilent Poroshell 120PFP column (150*4.6mm, 2.7μm), which was buffered with 0.01mol / L ammonium dihydrogen phosphate with a pH of 3.5 adjusted with phosphoric acid. The volume ratio of the solution and the organic phase was 50:50 as the mobile phase, the detection wavelength was 225 nm, the flow rate was 0.5 ml / min, the column temperature was 25 °C, the injection volume was 20 μl, and isocratic elution was performed.

[0060] The sample preparation is the same as in Example 1.

[0061] Test operation: Take 20 μl of system suitability solution and inject respectively, and record the chromatogram. The results are shown in Table 2.

[0062] Table 2 Summary table of organic phase screening results

[0063]

[0064] As can be seen from Table 2, either methanol or acetonitri...

Embodiment 3

[0065] Example 3 Comparison of mobile phase ratios

[0066] HPLC conditions:

[0067] The mobile phase ratios were tested respectively. The chromatographic column was an Agilent Poroshell 120PFP column (150*4.6mm, 2.7μm), and a mixture of 0.01mol / L ammonium dihydrogen phosphate buffer solution with a pH of 3.5 adjusted with phosphoric acid and acetonitrile was used. The solvent was the mobile phase, the detection wavelength was 225 nm, the flow rate was 0.5 ml / min, the column temperature was 25 °C, the injection volume was 20 μl, and isocratic elution was performed.

[0068] The sample preparation is the same as in Example 1.

[0069] Test operation: Take 20 μl of system suitability solution and inject respectively, and record the chromatogram. The results are shown in Table 3.

[0070] Table 3 Summary table of mobile phase ratio screening results

[0071]

[0072]

[0073] As can be seen from Table 2, when the volume ratio of ammonium dihydrogen phosphate buffer sol...

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Abstract

The invention discloses an analysis method for determining related substances in a glimepiride intermediate by utilizing HPLC (High Performance Liquid Chromatography), and particularly relates to an HPLC analysis method for the glimepiride intermediate and four impurities in the glimepiride intermediate. According to the present invention, with the chromatographic column type and specification, the detection wavelength, the mobile phase type, the mobile phase ratio, the operation time and the like, the impurities in the glimepiride intermediate can be rapidly, simply, accurately and efficiently eluted, separated and quantitatively detected, the complete separation between the impurity peak and the main peak and the complete separation between the impurities and the impurity peaks can be achieved, and the optimal detection result can be achieved; and the analysis method is convenient to operate, short in running time, high in specificity, sensitivity and stability, has a better linear curve in a low concentration range, has higher repeatability and accuracy, is not influenced by personnel and instruments, is stable and reliable, and provides a basis for research, development and quality detection of the compounds.

Description

technical field [0001] The invention belongs to the field of chemical drug analysis method development, in particular to an analysis method for related substances in a glimepiride intermediate. Background technique [0002] 4-[2-(3-ethyl-4-methyl-2-oxo-3-pyrroline-carboxamido)ethyl]benzenesulfonamide, CAS: 119018-29-0, its structural formula is as follows: [0003] [0004] Molecular formula: C 16 H 21 N 3 O 4 S molecular weight: 351.47 [0005] Glimepiride is a sulfonylurea antidiabetic drug, suitable for type 2 diabetes mellitus whose blood sugar cannot be adequately controlled by diet, exercise therapy and weight loss. It was first developed by the German company Hoechst Marion Roussel in the early 1980s. It was first listed in Germany and later in Switzerland, Sweden, Denmark and other countries. It was approved by the FDA in 1995 and launched in China in 2000. As a third-generation sulfonylurea hypoglycemic drug, glimepiride has the advantages of strong hypogl...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N30/86G01N30/02G01N30/06G01N30/34G01N30/36G01N30/60G01N30/74B01J20/281
Inventor 吴晓桐陆海波郭美丽王冉胡玉敬
Owner XUZHOU WANBANG JINQIAO PHARMA
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