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Method for separating and determining impurities in vitamin E and preparation thereof with HPLC (High Performance Liquid Chromatography) method

A vitamin and impurity technology, applied in drug analysis and detection, in the field of medicine, can solve the problems of cumbersome operation, poor reproducibility, harsh experimental conditions of gas chromatography, etc., and achieve the effect of high detection sensitivity and quality controllability

Active Publication Date: 2017-09-26
CHINESE MEDICINES GUANGZHOU
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0007] The detection methods for vitamin E impurities are currently only gas chromatography and titration, and high-performance liquid chromatography has not yet been retrieved for the detection of vitamin E impurities. Gas chromatography has harsh experimental conditions, cumbersome operations, and poor reproducibility. The detection of impurities is single, and the quality of vitamin E and its preparations cannot be effectively and comprehensively controlled

Method used

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  • Method for separating and determining impurities in vitamin E and preparation thereof with HPLC (High Performance Liquid Chromatography) method
  • Method for separating and determining impurities in vitamin E and preparation thereof with HPLC (High Performance Liquid Chromatography) method
  • Method for separating and determining impurities in vitamin E and preparation thereof with HPLC (High Performance Liquid Chromatography) method

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0036] Instrument: Waters high performance liquid chromatography;

[0037] Column: Wondasil C 18 Chromatographic column (250×4.6mm, 5μm);

[0038] Mobile Phase: Mobile Phase A: Acetonitrile-Ethanol-Water (35:10:55)

[0039] Mobile phase B: acetonitrile-ethanol-methanol (45:15:40);

[0040] Gradient elution program:

[0041] time (minutes)

Mobile phase A (%)

Mobile phase B (%)

0

20

80

110

20

80

112

10

90

140

10

90

142

20

80

150

20

80

[0042] Detection wavelength: 272nm;

[0043] Column temperature: 30°C

[0044] Flow rate: 1.0mL / min;

[0045] Preparation of dl-α-tocopherol acetate peak identification reference substance solution: Take about 7.5 mg of dl-α-tocopherol acetate peak identification reference substance, dissolve it in 5 ml of absolute ethanol, shake well, and obtain.

[0046]Preparation of vitamin E test solution: Take an appropriate amount of vitamin E raw material,...

Embodiment 2

[0054] Instrument: Waters high performance liquid chromatography;

[0055] Column: Wondasil C 18 Chromatographic column (250×4.6mm, 5μm);

[0056] Mobile phase: mobile phase A: acetonitrile-ethanol-water (40:10:50)

[0057] Mobile phase B: acetonitrile-ethanol-methanol (45:20:25);

[0058] Gradient elution program:

[0059] time (minutes)

Mobile phase A (%)

Mobile phase B (%)

0

25

75

110

25

75

112

0

100

140

0

100

142

25

75

150

25

75

[0060] Detection wavelength: 292nm;

[0061] Column temperature: 30°C

[0062] Flow rate: 1.0mL / min;

[0063] Solution preparation method and assay method are carried out according to " containing vitamin E preparation test sample solution " in embodiment 1, and the results are shown in Figure 5 .

Embodiment 3

[0065] Instrument: Waters high performance liquid chromatography;

[0066] Column: Wondasil C 18 Chromatographic column (250×4.6mm, 5μm);

[0067] Mobile Phase: Mobile Phase A: Acetonitrile-Ethanol-Water (40:15:45)

[0068] Mobile phase B: acetonitrile-ethanol-methanol (35:25:40);

[0069] Gradient elution program:

[0070] time (minutes)

Mobile phase A (%)

Mobile phase B (%)

0

15

85

110

15

85

112

5

95

140

5

95

142

15

85

150

15

85

[0071] Detection wavelength: 270nm;

[0072] Column temperature: 40°C

[0073] Flow rate: 1.1mL / min;

[0074] Solution preparation method and assay method are carried out according to " containing vitamin E preparation test sample solution " in embodiment 1, and the results are shown in Figure 6 .

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Abstract

The invention discloses a method for separating and determining impurities in vitamin E and a preparation thereof with an HPLC (High Performance Liquid Chromatography) method. The method comprises the following steps: chromatograph condition: by taking octadecylsilane bonded silica gel as filler, a mixed solution of acetonitrile, alcohol and water as a mobile phase A and a mixed solution of acetonitrile, alcohol and methanol as a mobile phase B, performing gradient elution, wherein a detection wavelength is 260-310nm, a column temperature is 25-45 DEG C, a flow rate of each mobile phase is 0.5-2.0mL / min, and a sample feeding quantity is 20-150 microlitres; preparation of a sample solution, adopting a polar solvent to prepare a d1-alpha-tocopherol acetate peak identification control solution with the concentration capable of being 0.5-3mg / mL; and determination: pouring the solution in a high performance liquid chromatograph, and recording and analyzing a chromatogram. By utilizing the method provided by the invention, quantitative analysis of related substances of the vitamin E as a crude drug and the preparation thereof can be accurately performed, and thus the quality controllability of the vitamin E and the preparation thereof is ensured.

Description

technical field [0001] The invention belongs to the technical field of medicine, in particular to the field of drug analysis and detection. The invention aims to establish a method for separating and measuring impurities in vitamin E and its related preparations by high performance liquid chromatography (HPLC method). Background technique [0002] Vitamin E is a fat-soluble vitamin, also known as tocopherol, anti-infertility vitamin, etc. It has a series of important physiological and biochemical functions such as anti-oxidation, reproduction, immunity, and anti-aging. It is an essential trace amount for animals and humans. Nutrients. This product is divided into synthetic or natural vitamin E, the synthetic type is (±)-2,5,7,8-tetramethyl-2-(4,8,12-trimethyltridecyl)-6 - chromanol acetate or dl - α -Tocopheryl acetate, natural form as (+)-2,5,7,8-tetramethyl-2-(4,8,12-trimethyltridecyl)-6-chroman Alcohol acetate or d - α - Tocopheryl acetate. The structural formula ...

Claims

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Application Information

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IPC IPC(8): G01N30/06G01N30/74
CPCG01N30/06G01N30/74
Inventor 邵爱霞孟祥娟王雅洁
Owner CHINESE MEDICINES GUANGZHOU
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