Method for authenticating dendrobium officinale by using HPLC fingerprint

A technology of Dendrobium officinale and fingerprint spectrum, which is applied in the field of establishment of fingerprints of Chinese medicinal materials, can solve the problems of staying, unfavorable to standardize the management of the traditional Chinese medicine industry, unable to realize the quality control of the medicinal materials of Dendrobium officinale, etc., and achieves the effects of easy operation and good reproducibility.

Inactive Publication Date: 2012-03-14
ZHEJIANG CHINESE MEDICAL UNIVERSITY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Some products marked as Dendrobium candidum (Fengdou) are not Dendrobium candidum, but other kinds of Dendrobium products, which damages the interests of consumers
In terms of quality control, the quality control of Dendrobium officinale in the 2010 edition of "Chinese Pharmacopoeia" still rests on the determination of properties and sugar content, which is far from achieving comprehensive quality control on Dendrobium officinale and is not conducive to the modernization of traditional Chinese medicine. and the standardization of industrial management

Method used

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  • Method for authenticating dendrobium officinale by using HPLC fingerprint
  • Method for authenticating dendrobium officinale by using HPLC fingerprint
  • Method for authenticating dendrobium officinale by using HPLC fingerprint

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0037] 1. Instruments and reagents

[0038] 1.1 Instrument: Agilent 1200 high performance liquid chromatograph; DAD detector.

[0039] 1.2 Reagents: Dendrobium officinale and its counterfeit products or substitutes are commercially available or provided by manufacturers; acetonitrile and methanol are chromatographically pure, and the rest of the reagents are analytically pure.

[0040] 2. Establishment of standard fingerprint of Dendrobium officinale medicinal materials

[0041] (1) Preparation of the test solution: Precisely weigh 10.0 g of fresh Dendrobium officinale medicinal materials, cut them into pieces, add 200 mL of water to reflux for extraction for 1 h, recover to a certain volume under reduced pressure, and extract with water-saturated n-butanol (20 mL*3 times), Recover n-butanol, dilute to volume with methanol, filter with 0.22 μm membrane, and use the filtrate as the test solution.

[0042] (2) Selection of chromatographic conditions: chromatographic separation...

Embodiment 2

[0047] The difference from Example 1 is:

[0048] Establishment of standard fingerprint of Dendrobium officinale:

[0049] (1) Preparation of the test solution: accurately weigh 2.0g of Dendrobium candidum, cut it into pieces, add 100mL of water to reflux for extraction for 1.5h, recover to a certain volume under reduced pressure, extract with ether (30mL*2 times), and recover ether , Methanol constant volume, 0.22μm membrane filtration, filtrate as the test solution.

[0050] (2) Selection of chromatographic conditions: the chromatographic separation column is SB-C18; the mobile phase is methanol-0.2% phosphoric acid; the gradient elution method is 0min→5min→12min→25min→40min→60min→70min; methanol 7%→14% →22%→30%→45%→55%→78%; flow rate 1.0mL / min; detection wavelength 270nm; column temperature 25°C; analyze the test solution under these conditions to obtain the fingerprint of Dendrobium candidum medicinal material.

Embodiment 3

[0052] The difference from Example 1 is:

[0053] Establishment of Standard Fingerprint of Dendrobium officinale

[0054] (1) Preparation of the test solution: Accurately weigh 1.0 g of Dendrobium candidum medicinal material powder, add 50 mL of methanol for ultrasonic extraction for 30 min, recover to a certain volume under reduced pressure, extract with ethyl acetate (20 mL*3 times), and recover ethyl acetate , Methanol constant volume, 0.45μm membrane filtration, filtrate as the test solution.

[0055] (2) Selection of chromatographic conditions: the chromatographic separation column is Xtimate TM C18; mobile phase is methanol-0.2% phosphoric acid; gradient elution method 0min→5min→10min→25min→45min→60min→75min; methanol 25%→25%→30%→40%→55%→70%→100 %; Flow rate 1.0mL / min; Detection wavelength 280nm; Column temperature 30°C; Analyze the test solution under this condition to obtain the fingerprint of Dendrobium candidum medicinal material.

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Abstract

The present invention provides a method for authenticating dendrobium officinale by using a HPLC fingerprint. The method comprises the following steps: (1) establishing a HPLC fingerprint of dendrobium officinale: a, precisely weighing powder of a dendrobium officinale medicinal material, adding water or a monohydric alcohol to carry out extraction and concentration, extracting by an organic solvent, carrying out treatments of recovering, concentrating, volume metering, filtering to obtain a tested sample solution; b, adopting a high performance liquid chromatography method to analyze the tested sample solution to obtain the fingerprint of the dendrobium officinale medicinal material; (2) establishing a standard fingerprint of the dendrobium officinale: carrying out analysis and comparison for 20 batches of the dendrobium officinale medicinal materials to obtain the standard fingerprint of the dendrobium officinale and the similarity of the dendrobium officinale medicinal material, wherein the similarity is more than 0.8; (3) adopting the same steps to detect the fingerprint of the dendrobium officinale counterfeit/substitute, carrying out comparison for the fingerprint of the dendrobium officinale counterfeit/substitute and the standard fingerprint of the dendrobium officinale, calculating the similarity, wherein the similarity is less than 0.6. According to the present invention, the standard fingerprint and the similarity can be adopted to effectively monitor the authenticity of the dendrobium officinale and the medicinal material quality.

Description

technical field [0001] The invention relates to a method for establishing fingerprints of Chinese medicinal materials, in particular to a method for identifying the authenticity of Dendrobium officinale medicinal materials by HPLC fingerprints, and provides a characteristic, accurate and simple modern identification method for the identification of Dendrobium officinale, which belongs to The field of pharmaceutical analysis technology. Background technique [0002] Dendrobium officinale is the dry stem of orchid Dendrobium officinale Kimura et MIgo. It has the functions of nourishing the stomach and promoting body fluid, nourishing yin and clearing away heat. It is mainly used in clinical treatment of yin injury and fluid loss, dry mouth and polydipsia, retching after eating less, irritability after illness, and dark eyesight. [0003] Dendrobium is an important traditional Chinese medicinal material in my country, and its medicinal value has been respected by people in the...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): A61K36/8984G01N30/02G01N30/36A61P43/00A61P1/02A61P1/14A61P1/08A61P27/10A61K135/00
Inventor 吕圭源周桂芬陈素红颜美秋
Owner ZHEJIANG CHINESE MEDICAL UNIVERSITY
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