Method for separating and determining glipizide and impurities thereof by liquid chromatography

A technology for glipizide and its determination method, which is applied in the field of separation and determination of glipizide and its impurities by high-performance liquid chromatography, and can solve the problems of poor peak shape of impurities, failure to achieve baseline separation, and influence on integral calculation, etc.

Active Publication Date: 2020-09-18
GUANGDONG HUANAN PHARMACEUTICAL GROUP CO LTD +2
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0018] The applicant found that the above method in the Pharmacopoeia can only partially separate and measure glipizide and its impurities, but the separation between some impurities is less than 1.5, which affects the integral calculation, and some impurities have poor peak shapes and have not reached the baseline separation. See the report on the simultaneous separation and determination of glipizide and the eleven impurities

Method used

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  • Method for separating and determining glipizide and impurities thereof by liquid chromatography
  • Method for separating and determining glipizide and impurities thereof by liquid chromatography
  • Method for separating and determining glipizide and impurities thereof by liquid chromatography

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0078] Instrument: Agilent 1260 InfinityII;

[0079] Stationary phase: Agilent ZORBAX SB-C18 (4.6mm×150mm, 5μm);

[0080] mobile phase:

[0081] Phase A: 0.015mol / L potassium dihydrogen phosphate, adjust the pH value to 3.7 with phosphoric acid;

[0082] Phase B: acetonitrile;

[0083] Phase C: Methanol;

[0084] Column temperature: 25°C;

[0085] Injection volume: 20μL;

[0086] Flow rate: 1.0mL / min;

[0087] Detection wavelength: 225nm;

[0088] Preparation of mobile phase:

[0089] Phase A: Take 2.04g of potassium dihydrogen phosphate, add water to dissolve and dilute to 1000mL, adjust the pH value to 3.7 with phosphoric acid;

[0090] Phase B: acetonitrile;

[0091] Phase C: Methanol.

[0092] Mobile phase gradient settings:

[0093] stage V A相 (％)

V B相 (％)

V C相 (％)

Elution time 0 65 25 10 7min 1 50 30 20 5min 2 40 35 25 6min 3 30 45 25 6min

[0094] Solution preparation:

[0095] Diluent: 0.015mol / L ...

Embodiment 2

[0101] Instrument: Agilent 1260 InfinityII;

[0102] Stationary phase: Agilent ZORBAX SB-C18 (4.6mm×150mm, 5μm);

[0103] mobile phase:

[0104] Phase A: 0.010mol / L potassium dihydrogen phosphate, adjust the pH value to 3.5 with phosphoric acid;

[0105] Phase B: acetonitrile;

[0106] Phase C: Methanol;

[0107] Column temperature: 20°C;

[0108] Injection volume: 15μL;

[0109] Flow rate: 0.8mL / min;

[0110] Detection wavelength: 225nm;

[0111] Preparation of mobile phase:

[0112] Phase A: Take 1.36g of potassium dihydrogen phosphate, add water to dissolve and dilute to 1000mL, adjust the pH value to 3.5 with phosphoric acid;

[0113] Phase B: acetonitrile;

[0114] Phase C: Methanol.

[0115] Mobile phase gradient settings:

[0116] stage V A相 (％)

[0117] Solution preparation method and assay method are carried out with reference to embodiment 1, record chromatogram figure 2 . The chromatographic conditions of this embodiment can effectively disti...

Embodiment 3

[0119] Instrument: Agilent 1260 Infinity II;

[0120] Stationary phase: Agilent ZORBAX SB-C18 (4.6mm×150mm, 5μm);

[0121] mobile phase:

[0122] Phase A: 0.018mol / L potassium dihydrogen phosphate, adjust the pH value to 4.0 with phosphoric acid;

[0123] Phase B: acetonitrile;

[0124] Phase C: Methanol;

[0125] Column temperature: 30°C;

[0126] Injection volume: 30μL;

[0127] Flow rate: 1.2mL / min;

[0128] Detection wavelength: 225nm;

[0129] Preparation of mobile phase:

[0130] Phase A: Take 2.45g of potassium dihydrogen phosphate, add water to dissolve and dilute to 1000mL, add phosphoric acid to adjust the pH to 4.0;

[0131] Phase B: acetonitrile;

[0132] Phase C: Methanol.

[0133] Mobile phase gradient settings:

[0134] stage V A相 (％)

[0135] Solution preparation method and assay method are carried out with reference to embodiment 1, record chromatogram image 3 . The chromatographic conditions of this embodiment can effectively distingui...

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Abstract

The invention discloses a method for separating and determining glipizide and impurities thereof through high performance liquid chromatography and application. According to the determination method,a chromatographic column taking octadecylsilane chemically bonded silica as a filler is adopted; detection conditions are as follows: chromatographic conditions: the chromatographic column is an octadecylsilane chemically bonded silica chromatographic column; the mobile phase is 0.010 to 0.018 mol / L monopotassium phosphate-acetonitrile-methanol, and the pH value is adjusted to 3.5 to 4.0 by usingphosphoric acid; the column temperature is 20 to 30 DEG C; the sample injection amount is 15 to 30 mu L; the sample injection concentration is 0.0003 to 2 mg / mL; the flow rate is 0.8 to 1.2 mL / min; and the detection wavelength is 225 nm, and gradient elution is carried out. The method disclosed by the invention is high in precision, good in repeatability and high in recovery rate, and can be widely applied to quality detection of glipizide bulk drugs with different sources and corresponding preparations of the glipizide bulk drugs.

Description

technical field [0001] The invention belongs to the field of drug analysis, and in particular relates to a method for separating and measuring glipizide and its impurities through high-performance liquid chromatography. Background technique [0002] Glipizide, a second-generation sulfonylurea oral hypoglycemic agent, is suitable for patients with mild to moderate type II diabetes mellitus who are unsatisfied with diet control and physical exercise. The chemical formula of glipizide is 1-cyclohexyl-3-{4-[2-(5-methylpyrazine-2-amide)-ethyl]benzenesulfonyl}urea, and the molecular formula is C 21 h 27 N 5 o 4 S, molecular weight is 445.54, the structural formula of glipizide is: [0003] [0004] During the production and storage of glipizide, the purity of the drug may be affected due to incomplete removal of starting materials and intermediates and degradation impurities generated during storage. These substances that affect the purity of the drug are called related sub...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N30/88
CPCG01N30/88G01N2030/884
Inventor 程志伟顾云林艾瑜郑艳芳
Owner GUANGDONG HUANAN PHARMACEUTICAL GROUP CO LTD
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