High performance liquid chromatography method for determining nicergoline related substances

A high-performance liquid chromatography and nicergoline technology, applied in the field of drug analysis, can solve the problems of unstable retention time of impurities, difficulty in obtaining impurity reference substances, and high price of impurity reference substances

Active Publication Date: 2018-09-28
CHONGQING INST FOR FOOD & DRUG CONTROL
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The gradient elution method is greatly affected by factors such as reagents, chromatographic columns, and the brand and model of high-performance liquid chromatography, resulting in unstable relative retention times of impurities. Therefore, each test needs to be positioned with an impurity reference substance, which is expensive and expensive. Not easy to get
At present, there is no isocratic elution high-efficiency liquid that can not only accurately determine the content of impurity D, but also simultaneously determine the known impurities C, B, A, G, F, H and other unknown impurities of Nicergoline by the relative retention time method. phase chromatography

Method used

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  • High performance liquid chromatography method for determining nicergoline related substances
  • High performance liquid chromatography method for determining nicergoline related substances
  • High performance liquid chromatography method for determining nicergoline related substances

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0074] The verification of embodiment 1 chromatographic conditions

[0075] Chromatographic column: Filler with a mixture of strong cation exchange resin and reverse phase C18 in a volume ratio of 1:4;

[0076] Mobile phase: Acetonitrile is used as mobile phase A, and phosphate buffer (60 mmol / L potassium dihydrogen phosphate solution containing 0.5% triethylamine, adjusted to pH 2.1 with phosphoric acid) is used as mobile phase B. The ratio of mobile phase A and mobile phase B is 30:70 for isocratic elution;

[0077] Detection wavelength: 288nm;

[0078] Column temperature: 30°C;

[0079] Preparation of impurity test solution: take one EP system applicability reference substance, add 1ml of acetonitrile to dissolve it, and get it;

[0080] The preparation of mixed impurity reference substance solution: get impurity D 9.42mg, impurity A (lonyergoline) 10.68mg, impurity G (1-desmethoxynicergoline) 10.25mg, impurity B (1-norniergoline) ) 10.30mg, impurity C 10.30mg, put in 1...

Embodiment 2

[0085] The thermal stability investigation of embodiment 2 Nicergoline

[0086] Accurately weigh 0.1028g of the Nicergoline reference substance, put it in a 100ml measuring bottle, add acetonitrile-water (8:2) to dissolve and dilute to the mark, shake well, and use it as the test solution. Take the test solution and heat it in a water bath at 60°C to destroy it, and accurately measure 20 μl of the test solution heated for 0 min, 10 min, 30 min, and 50 min respectively and inject it into the liquid chromatograph, record the chromatogram according to the chromatographic conditions in Example 1, see Figure 4~7 , the results showed that Nicergoline was thermally degraded, and impurity D and impurity C gradually increased with heating time, see Table 1 for details.

[0087] Table 1

[0088]

Embodiment 3

[0089] Embodiment 3 linear range, detection limit and quantitative limit

[0090] Take impurity D 9.42mg, impurity A (lonyergoline) 10.68mg, impurity G (1-desmethoxynicergoline) 10.25mg, impurity B (1-norniergoline) 10.30mg, impurity C 10.30, Nicergoline reference substance 10.12 mg was put in a 10ml measuring bottle respectively, dissolved with acetonitrile and diluted to the mark as each reference substance stock solution. Accurately measure an appropriate amount of each reference substance stock solution, dilute with acetonitrile to make a series of solutions, and accurately measure 10 μL respectively according to the chromatographic conditions of Example 1 and inject it into a liquid chromatograph, and record the chromatogram. In concentration (μg·ml -1 ) is x, and taking the peak area as y, calculate the linear regression equation and the correction factor (the ratio of the slope of Nicergoline to the slope of each component) of each component respectively, the results a...

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Abstract

The invention belongs to the field of medicine analysis, and particularly relates to a high performance liquid chromatography method for determining nicergoline related substances. According to the high performance liquid chromatography method, a filler obtained by mixing strong cation exchange resin and a reversed phase C18 according to a volume ratio of 1 to 4 is used as a filling agent, acetonitrile is used as a mobile phase A, a phosphate buffer is used as a mobile phase B, the mobile phase A and the mobile phase B are mixed according to a ratio of 30 to 70 for isocratic elution, the detection wavelength is 288nm, and the column temperature is 30 DEG C. By the high performance liquid chromatography method, the content of an impurity D can be accurately determined and known impurities C, B, A, G, F and H and other unknown impurities in nicergoline can be simultaneously determined.

Description

technical field [0001] The invention belongs to the field of drug analysis, in particular to a high performance liquid chromatography method for determining nicergoline related substances. Background technique [0002] Nicergoline is a semi-synthetic ergot alkaloid derivative, which has α-receptor blocking effect and vasodilator effect, can strengthen the energy metabolism of brain cells, and is suitable for acute and chronic cerebrovascular and peripheral circulation disorders, brain metabolic dysfunction and Headache, rapidly absorbed after oral administration. Impurity D (5-bromopyridine-3-carboxylic acid) and impurity C (methyl phoergoline) are the raw materials for the synthesis of Nicergoline, and are also its main degradation products, which exist in Nicergoline raw materials, especially in preparations . For example, Nicergoline undergoes technical steps such as granulation and drying in the production process of the preparation, and the raw material of Nicergoline...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N30/06G01N30/74
CPCG01N30/06G01N30/74
Inventor 周琳程辉跃黄俊曾令高陈竹张迪梁静王益平
Owner CHONGQING INST FOR FOOD & DRUG CONTROL
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