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

A determination method and high-performance liquid chromatography technology are applied in the field of high-performance liquid chromatography for the separation and determination of berberine and its impurities, and can solve the problems that simultaneous separation and determination of berberine cannot be achieved, high sensitivity, and wide linear range.

Active Publication Date: 2020-09-01
GUANGDONG HUANAN PHARMACEUTICAL GROUP CO LTD +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The applicant found that the above patents or documents can only partially separate and measure berberine and its impurities, but cannot achieve simultaneous separation and determination of berberine and the nine impurities, and there is no simultaneous separation of berberine and the nine impurities Determination method, the present invention starts from the deficiencies of the prior art, and provides an analysis method, which can accurately and rapidly separate and measure berberine and the nine impurities, and the method has high sensitivity and a wide linear range, and plays a role in daily production. Control the quality of berberine, improve the efficacy of medicines, and reduce toxic and side effects

Method used

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

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0077] Instrument: Agilent 1260 Infinity II;

[0078] Stationary phase: YMC Triart C18 chromatographic column (4.6mm×150mm, 3μm);

[0079] mobile phase:

[0080] Phase A: 0.05mol / L ammonium dihydrogen phosphate-1.0% triethylamine, adjust the pH value to 3.2 with phosphoric acid;

[0081] Phase B: acetonitrile;

[0082] Column temperature: 25°C;

[0083] Injection volume: 10μL;

[0084] Flow rate: 1.0mL / min;

[0085] Detection wavelength: 236nm;

[0086] Preparation of mobile phase:

[0087] Phase A: Take 5.75g of ammonium dihydrogen phosphate, add water to dissolve and dilute to 1000mL, add 1.0% triethylamine and then add phosphoric acid to adjust the pH value to 3.2;

[0088] Phase B: acetonitrile.

[0089] Mobile phase gradient settings:

[0090]

[0091]

[0092] Solution preparation:

[0093] Blank solvent: 0.05mol / L ammonium dihydrogen phosphate solution (containing 1.0% triethylamine, adjust the pH value to 3.2-acetonitrile (77:23) with phosphoric acid (t...

Embodiment 2

[0112] Instrument: Agilent 1260 Infinity II;

[0113] Stationary phase: YMC Triart C18 chromatographic column (4.6mm×150mm, 3μm);

[0114] mobile phase:

[0115] Phase A: 0.03mol / L ammonium dihydrogen phosphate-1.0% triethylamine, adjust the pH value to 3.0 with phosphoric acid;

[0116] Phase B: acetonitrile;

[0117] Column temperature: 23°C;

[0118] Injection volume: 5 μL;

[0119] Flow rate: 0.8mL / min;

[0120] Detection wavelength: 236nm;

[0121] Preparation of mobile phase:

[0122] Phase A: Take 3.45g of ammonium dihydrogen phosphate, add water to dissolve and dilute to 1000mL, add 1.0% triethylamine and then add phosphoric acid to adjust the pH value to 3.0;

[0123] Phase B: acetonitrile.

[0124] Mobile phase gradient settings:

[0125] stage V A相 :V B相

[0126] 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 e...

Embodiment 3

[0128] Instrument: Agilent 1260 Infinity II;

[0129] Stationary phase: YMC Triart C18 chromatographic column (4.6mm×150mm, 3μm);

[0130] mobile phase:

[0131] Phase A: 0.08mol / L ammonium dihydrogen phosphate-1.0% triethylamine, adjust the pH value to 3.5 with phosphoric acid;

[0132] Phase B: acetonitrile;

[0133] Column temperature: 28°C;

[0134] Injection volume: 15μL;

[0135] Flow rate: 1.2mL / min;

[0136] Detection wavelength: 236nm;

[0137] Preparation of mobile phase:

[0138] Phase A: Take 9.20 g of ammonium dihydrogen phosphate, add water to dissolve and dilute to 1000 mL, add 1.0% triethylamine and then add phosphoric acid to adjust the pH value to 3.5;

[0139] Phase B: acetonitrile.

[0140] Mobile phase gradient settings:

[0141] stage V A相 :V B相

[0142] 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 ...

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Abstract

The invention discloses a method for separating and determining berberine 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 0.03-0.08 mol / L ammonium dihydrogen phosphate-acetonitrile, the pH value of the mobile phase is 3.0-3.5, the column temperature is 23-28 DEG C, the sample injection amount is 5-15 microliters, the sample injection concentration is 0.0005-2 mg / mL, the flow rate is 0.8-1.2 mL / min, the detection wavelength is 236 nm, andgradient elution is performed. The method is high in precision, good in repeatability and high in recovery rate, and can be widely applied to quality detection of berberine bulk drugs from different sources and corresponding preparations thereof.

Description

technical field [0001] The invention belongs to the field of drug analysis, in particular to a method for separating and measuring berberine and its impurities through high-performance liquid chromatography. Background technique [0002] Berberine (Berberine) is the main isoquinoline alkaloid in the stems and roots of various Berberine plants. To treat a range of diseases such as intestinal infections, gastroenteritis, etc. The chemical formula of berberine is 5,6-dihydro-9,10-dimethoxybenzo[g]-1,3-benzodioxolane[5,6-α]quinazine, and the molecular formula is C 20 h 18 NO 4 , the molecular weight is 336.37, and the structural formula of berberine is: [0003] [0004] During the production and storage of berberine, 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 substances. The above-mentio...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N30/02G01N30/34
CPCG01N30/02G01N30/34
Inventor 顾云程志伟杨晓敏
Owner GUANGDONG HUANAN PHARMACEUTICAL GROUP CO LTD
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