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Method for measuring content of kaempferol-3-O-rutinoside in radix tetrastigme medicinal material

A determination method and rutinoside technology are applied in the field of determination of the content of kaempferol-3-O-rutinoside in Sanyeqing medicinal materials, which can solve the problems of large amount of extraction solvent, cumbersome determination method, large sample sampling amount, etc. The measurement method is simple and fast, the sampling amount is small, and the effect of less dosage

Pending Publication Date: 2020-08-07
TONGDE HOSPITAL OF ZHEJIANG PROVINCE
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

When using high-performance liquid chromatography to measure the flavonoids in Clover, because there are many types of flavonoids in Clover, the required sample sampling volume is relatively large, which is 3.0-4.0g; the amount of extraction solvent is large, which is 40-50mL. Moreover, the solution needs to be concentrated after extraction, and the determination method is relatively cumbersome.

Method used

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  • Method for measuring content of kaempferol-3-O-rutinoside in radix tetrastigme medicinal material
  • Method for measuring content of kaempferol-3-O-rutinoside in radix tetrastigme medicinal material
  • Method for measuring content of kaempferol-3-O-rutinoside in radix tetrastigme medicinal material

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preparation example Construction

[0049] In the present invention, the trifoliate green powder is mixed with methanol, followed by ultrasonic extraction and microfiltration, and the filtrate obtained by the microfiltration is the test solution. In the present invention, the preparation method of the Clover powder preferably comprises the following steps:

[0050] The cloverleaf medicinal material is sequentially crushed and sieved to obtain the cloverleaf powder.

[0051] The present invention has no special requirements on the pulverization method, and the pulverization method well known to those skilled in the art can be used. In the present invention, the sieving is preferably a 40-60 mesh sieve, and the particle size of the Clover powder is preferably ≥ 40 mesh, more preferably ≥ 60 mesh.

[0052] In the present invention, the mass of the Clover powder is 0.11-0.22g, preferably 0.2g; the volume of the methanol is 5-10mL, preferably 10mL. In the present invention, there is no special requirement on the mi...

Embodiment 1

[0086] Exclusive experiment:

[0087] (1) Accurately weigh 1.6 mg of kaempferol-3-O-rutinoside reference substance (purchased from Chengdu Aifa Biotechnology Co., Ltd., batch number: AF8112493, purity: 98%), dissolve in methanol and dilute to 1 mL, take Put 0.25ml in a 10mL volumetric flask and add methanol to the volume, then take 1mL of the solution to a 10mL volumetric flask and add methanol to the volume to obtain a kaempferol-3-O-rutinoside reference solution with a concentration of 0.004mg / mL.

[0088] (2) Take an appropriate amount of decoction pieces of Clover, crushed, passed through a 60-mesh sieve, weighed 0.2g of Clover powder, weighed accurately, placed in a 10mL volumetric flask, added methanol to constant volume, sealed, and ultrasonicated (power: 400W , frequency: 40kHz) 60min, let cool to room temperature, make up the loss with methanol, take the solution and filter it with an alcohol-soluble 0.45μm microporous membrane, and take the continued filtrate as the ...

Embodiment 2

[0096] (1) Take an appropriate amount of decoction pieces of Clover, crush them, pass through a 60-mesh sieve, weigh 0.2g of Clover powder, weigh it accurately, put it in a 10mL volumetric flask, add methanol to the volume, seal it, and ultrasonic (power: 400W , frequency: 40kHz) 60min, let cool to room temperature, make up the loss with methanol, take the solution and filter it with an alcohol-soluble 0.45μm microporous membrane, and take the filtrate as the test solution.

[0097] (2) 10 μ L of need testing solution is carried out high performance liquid chromatography analysis, and analysis parameter is identical with embodiment 1, and gained HPLC collection of illustrative plates is as follows Figure 9 as shown, Figure 9 The peak at 21.451min in the center is the kaempferol-3-O-rutinoside peak, and the mass percentage composition of kaempferol-3-O-rutinoside in the Clover Green powder is calculated by regression equation and formula I and formula II as 0.00927%.

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Abstract

The invention provides a method for determining the content of kaempferol-3-O-rutinoside in a radix tetrastigme medicinal material, and belongs to the technical field of chemical detection. Accordingto the method, the content of kaempferol-3-O-rutinoside in the radix tetrastigme medicinal material is determined through high performance liquid chromatography, the sampling amount is small, the dosage of an extraction solvent is small, an extraction solution does not need to be concentrated, the determination method is simple, convenient, rapid and good in repeatability, and the quality of the radix tetrastigme medicinal material can be accurately evaluated. The result of the embodiment shows that the separation degree of the kaempferol-3-O-rutinoside peak and other peaks in the spectrogramobtained by the method is greater than 1.5, which shows that the separation degree is good; in a linear relation test, the linear relation of the sample size of the determination method disclosed by the invention is good in a range of 0.004-0.12 [mu] g; in a repeatability test, the relative standard deviation of the content of kaempferol-3-O-rutinoside in the determination method is 2.76%, which indicates that the method provided by the invention has good repeatability.

Description

technical field [0001] The invention relates to the technical field of production of pharmaceutical intermediates, in particular to a method for determining the content of kaempferol-3-O-rutinoside in the trifolium medicinal material. Background technique [0002] Clover (Tetrastigma hemsleyanum Diels et Gilg) is a perennial evergreen vine belonging to the family Vitis genus, and it is a unique rare medicinal plant in my country. Clover has the effects of clearing heat and detoxifying, reducing swelling and relieving pain, resolving phlegm and resolving stagnation, and is used to treat febrile convulsions, pneumonia, hepatitis, snake bites and other diseases. Clover is mainly distributed in Zhejiang, Jiangxi, Fujian, Hunan, Guangxi, Guizhou and other places. [0003] At present, the quality control components of Clover are the flavonoids in Clover. When using high-performance liquid chromatography to measure the flavonoids in Clover, because there are many types of flavono...

Claims

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Application Information

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IPC IPC(8): G01N30/02G01N30/34G01N30/74
CPCG01N30/02G01N30/34G01N30/74
Inventor 李洪玉张红心李礼斌王娜妮许平翠寿旦
Owner TONGDE HOSPITAL OF ZHEJIANG PROVINCE
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