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Method for detecting content of various biflavones in ginkgo leaf preparation

A technology of ginkgo biloba and biflavone, which is applied in the field of content determination of traditional Chinese medicine preparations, can solve the problems of long time consumption and low detection sensitivity, and achieve the effects of shortening detection time, controlling safety, and saving detection time and cost

Inactive Publication Date: 2018-05-11
ZHEJIANG WANBANG PHARMA
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

At the same time, the import standard of ginkgo leaf extract also stipulates that the content of ginkgo biflavonoids should be controlled within 0.1%. The detection method is aimed at the total biflavones, which takes a long time and has low detection sensitivity.
At present, there is no limit standard in the pharmacopoeia standards of domestic ginkgo biloba preparations. It is clear that the specific content of various biflavones plays an important role in improving the quality of ginkgo biloba preparations and is related to the drug safety of patients.

Method used

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  • Method for detecting content of various biflavones in ginkgo leaf preparation
  • Method for detecting content of various biflavones in ginkgo leaf preparation
  • Method for detecting content of various biflavones in ginkgo leaf preparation

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0066] (1) High performance liquid chromatography conditions

[0067] Instrument: HPLC (Waters e2695);

[0068] Chromatographic system: Chromatographic column: Welch Bolimate C18 (100mm×3mm, 2.7μm);

[0069] Detection wavelength: 330nm; column temperature: 30°C; injection volume: 20μl; detector sensitivity: 0.04AUFS;

[0070] Mobile phase: flow rate 0.5ml / min.

[0071] The elution conditions are 0 minutes, 30% A; 0-20 minutes, 30%-45% A; 20-25 minutes, 45%-100% A; 25-30 minutes, 100%-30% A; 30-35 Minutes, 30% A.

[0072] (2) Preparation of standard solution:

[0073] (a) Standard product solution of Biflavones of P. chinensis: Accurately weigh 2mg of A. flavonoids of P. chinensis standard, dissolve them in 2ml of DMSO, shake well, take 1ml and dilute to 200ml with chromatographic methanol, and make 5.320μg / ml Abiflavones of P. chinensis Standard solution.

[0074] (b) Ginkgo biflavone standard solution: Accurately weigh 2mg of Ginkgo biflavone standard substance, dissolv...

Embodiment 2

[0086] The difference from Example 1 is that the chromatographic column is: AgilentC18 (250mm×4.6mm, 5 μm); mobile phase: acetonitrile (A)-water (B) solution, gradient elution, the elution condition is 0 to 30 minutes, 47 %A; 30-33 minutes, 47%-80%A; 33-42 minutes, 80%A; 42-45 minutes, 80%-47%A; 45-55 minutes, 47%A; flow rate 1.0ml / min ; Detection wavelength: 270nm; Column temperature 40°C.

Embodiment 3

[0088] The same batch of Ginkgo Leaf Dropping Pills was used to verify the method of Example 1, and the sample solutions to be tested were respectively obtained for the determination of the biflavone content, and the precision was investigated. The results are shown in Table 3. The results showed that the RSD of assay met the requirement of RSD within 3%.

[0089] Table 3 The inventive method repeatability experiment content determination (unit: ppm)

[0090]

[0091] In the methodological verification of this method, the accuracy investigation (recovery rate experiment) meets the range requirements of 95% to 105%, and the RSD meets the requirements within 5%.

[0092] Experimental operation is the same as embodiment 1, and the results are shown in Table 4.

[0093] Table 4 The inventive method accuracy measurement

[0094]

[0095]

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Abstract

The invention discloses a method for detecting the content of various biflavones in a ginkgo leaf preparation. The method can detect amentoflavone, ginkgetin, isoginkgetin, bilobetin and sciadopitysinin the ginkgo leaf preparation simultaneously, an HPLC(Waters e2695) and Welch Bolimate C18 column is adopted for determination; a mobile phase is acetonitrile-water, and gradient elution is conducted, wherein the volume fraction of acetonitrile is 40%-80%, the flow velocity is 0.5 ml / min, the detection wavelength is 330 nm, and the column temperature is 30 DEG C; automatic sample introduction isconducted on standard substances and samples for test separately, and the content of five biflavones is calculated with an external standard method. Accordingly, by means of detection of the biflavone content, the quality control standard of the ginkgo leaf preparation is greatly improved; complex pretreatment is not needed, rapid detection can be achieved, the detection time is saved, and the detection cost is reduced.

Description

Technical field: [0001] The invention relates to a method for determining the content of traditional Chinese medicine preparations, in particular to a method for detecting the contents of multiple biflavones in ginkgo biloba preparations. technical background: [0002] Ginkgo biloba L. is a relict plant that survived on the earth during the Ice Age and is known as a "living fossil". China is the birthplace of ginkgo, and its resources account for about 70% of the world's total. At present, Germany, France, and the United States have become the three major sales markets for ginkgo biloba extracts, while in Asia, the sales of ginkgo biloba extracts in Japan, China, and South Korea are the best. [0003] Ginkgo biloba has anti-oxidation, scavenging free radicals in the body, anti-platelet activating factors, reducing blood viscosity, improving microcirculation, improving memory, increasing cerebral blood flow, protecting cerebral microvascular smooth muscle cells, reducing bra...

Claims

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Application Information

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IPC IPC(8): G01N30/02
CPCG01N30/02
Inventor 陈莉王青青张瑶丹杨韬炜陈奕聪
Owner ZHEJIANG WANBANG PHARMA
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