Method for establishing fingerprint spectrum of flavonoid components in ginkgo leaf extraction intermediate or preparation thereof and fingerprint spectrum established by method

A technology of fingerprint spectrum and establishment method, which is applied in the field of fingerprint spectrum, the establishment of the fingerprint spectrum of flavonoids in Ginkgo biloba extract intermediates or their preparations, can solve the problems of not truly and comprehensively reflecting the flavonoids, and achieves easy identification, Monitor quality, peak shape is good

Active Publication Date: 2021-08-13
HEILONGJIANG ZBD PHARMA +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Therefore, the fingerprints disclosed in the patent application documents do not truly and comprehensively reflect the flavonoid components of Ginkgo biloba extract or its preparations

Method used

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  • Method for establishing fingerprint spectrum of flavonoid components in ginkgo leaf extraction intermediate or preparation thereof and fingerprint spectrum established by method
  • Method for establishing fingerprint spectrum of flavonoid components in ginkgo leaf extraction intermediate or preparation thereof and fingerprint spectrum established by method
  • Method for establishing fingerprint spectrum of flavonoid components in ginkgo leaf extraction intermediate or preparation thereof and fingerprint spectrum established by method

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0258] Example 1 Choice of detection wavelength

[0259] UV full-wavelength scanning of representative pinoresinol diglucoside and flavonoids representative of lignans in the intermediate of Ginkgo biloba extract, see figure 1 .

[0260]Preparation of quercetin reference substance solution: Accurately weigh an appropriate amount of quercetin reference substance, dilute it with 50% (v / v) methanol aqueous solution to a solution containing 0.012 mg per 1 ml, shake well, and obtain.

[0261] Preparation of pinoresinol diglucoside reference substance solution: Accurately weigh an appropriate amount of pinoresinol diglucoside reference substance, dilute with 50% (v / v) methanol aqueous solution to a solution containing 44.6 μg per 1 ml, shake well, and obtain.

[0262] From figure 1 It can be seen that the flavonoids present a characteristic maximum absorption wavelength near 360nm (see figure 1 B below); lignans do not absorb at 360nm but absorb at 265nm (see figure 1 A) above...

Embodiment 2

[0263] Example 2 Column Selection

[0264] Preparation of the test sample: Accurately measure 2ml of Shuxuening injection, put it in a 10ml measuring bottle, dilute to the mark with 50% (v / v) aqueous methanol solution, shake well, filter, and take the subsequent filtrate to obtain final product.

[0265] Chromatographic conditions: Acetonitrile was used as phase A, 0.1% (v / v) formic acid aqueous solution was used as phase B, and the gradient elution program was shown in Table 1.

[0266] Table 1 Gradient elution program (volume percentage)

[0267] time (min) Acetonitrile (%) 0.1% formic acid aqueous solution (%) 0 18 82 12 21 79 15 25 75 25 35 65

[0268] Flow rate 0.25ml / min;

[0269] Column temperature: 35°C;

[0270] Detection wavelength: 360nm;

[0271] Injection volume: 1 μl.

[0272] (1) Column 1

[0273] Model: Agilent ZORBAX SB-C18 (3.0×150 mm, 1.8 μm).

[0274] Chromatogram see figure 2 A.

[0275] (2) Column 2

...

Embodiment 3

[0283] Example 3 Choice of mobile phase

[0284] The method for preparing need testing solution according to embodiment 2, chromatographic column is Agilent ZORBAX SB-C18 (3.0 * 150mm, 1.8 μ m), other chromatographic conditions are the same as embodiment 2 except mobile phase.

[0285] (1) Mobile phase: acetonitrile-water

[0286] The gradient elution program is shown in Table 2.

[0287] Table 2 Acetonitrile-water gradient elution program (volume percentage)

[0288] time (min) Acetonitrile (%) water(%) 0 18 82 12 21 79 15 25 75 25 35 65

[0289] Chromatogram see image 3 A above.

[0290] (2) mobile phase methanol-water

[0291] Using methanol-water mobile phase, the system pressure is high, which is close to the maximum pressure of the chromatographic column, so it is not suitable to use methanol-water as the mobile phase.

[0292] (3) mobile phase acetonitrile-0.1% formic acid aqueous solution

[0293] The gradient elution...

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Abstract

The invention provides a method for establishing a fingerprint spectrum of flavonoid components in a ginkgo leaf extraction intermediate or a preparation thereof and the fingerprint spectrum established by the method. The method for establishing the fingerprint spectrum comprises the step of detecting the relative retention time and / or the relative peak area of flavonoid components in the ginkgo leaf extraction intermediate or the preparation thereof by taking narcissoside as a reference and adopting a high performance liquid chromatography. The fingerprint spectrum comprises 23 common peaks. The invention also provides an application of the the method for establishing the fingerprint spectrum and / or the established fingerprint in true and false identification and component detection of the ginkgo leaf extraction intermediate and / or the preparation thereof.

Description

technical field [0001] The invention belongs to the fields of analytical chemistry and drug quality control, and in particular relates to a method for establishing fingerprints of flavonoid components in ginkgo leaf extraction intermediates or preparations thereof and the established fingerprints. Background technique [0002] Ginkgo biloba is the dried leaf of Ginkgo biloba (Ginkgo biloba L.), sweet, bitter, astringent, flat, heart-guiding, and lung meridian. Ginkgo biloba extract intermediate is the extract / liquid processed by Ginkgo biloba, which is widely used in medicine, health products, food additives, functional beverages, cosmetics and other fields, and is the most successful botanical medicine developed by modern science and technology. Case one. Shuxuening injection is a sterilized aqueous solution made from the intermediate of Ginkgo biloba extract, which is used for ischemic cardiovascular and cerebrovascular diseases, coronary heart disease, angina pectoris, c...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N30/06G01N30/74G01N30/86
CPCG01N30/06G01N30/74G01N30/8686
Inventor 方同华王春生林珊佟美鸿刘玉成姚洪艳武志立董丽丽
Owner HEILONGJIANG ZBD PHARMA
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