Method for establishing rhizoma bletillae high performance liquid chromatography (HPLC) fingerprint spectrum and standard fingerprint spectrum thereof

A technology of high performance liquid chromatography and standard fingerprint spectrum, which is applied in measurement devices, instruments, scientific instruments, etc., can solve problems such as difficulty in objectively and effectively evaluating or controlling the quality of medicinal materials, and achieves simple production, stability and reproducibility. Good, easy chromatographic conditions

Inactive Publication Date: 2013-10-09
GUANGZHOU UNIVERSITY OF CHINESE MEDICINE
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  • Abstract
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AI Technical Summary

Problems solved by technology

Although there are successive literatures on the content determination of chemical components in white and Chinese medicine, including cinnamic acid, 2,7-dihydroxy-4-methoxy-9,10-dihydrophenanthrene, 2,4-dimethoxy-3,7 -Dihydroxyphenanthrene, total phenols, and total polysaccharides, but for Chinese herbal medicines such as Baiji, which have many types of active ingredients and complex components, it is difficult to objectively and effectively evaluate or control the quality of medicinal materials by only measuring the content of certain types of ingredients
However, there is no report on the testing and analysis of white and fingerprints using high performance liquid chromatography (HPLC)

Method used

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  • Method for establishing rhizoma bletillae high performance liquid chromatography (HPLC) fingerprint spectrum and standard fingerprint spectrum thereof
  • Method for establishing rhizoma bletillae high performance liquid chromatography (HPLC) fingerprint spectrum and standard fingerprint spectrum thereof
  • Method for establishing rhizoma bletillae high performance liquid chromatography (HPLC) fingerprint spectrum and standard fingerprint spectrum thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0040] Embodiment 1: the preparation of need testing solution

[0041] (1) Selection of extraction solvent

[0042] According to literature search, ethanol and methanol are commonly used solvents for fingerprint research. Therefore, methanol and ethanol were used as extraction solvents to extract the white powder and its decoction pieces, and the extraction efficiencies of the main components in the white powder were compared between the two solvents.

[0043] Sample treatment: Accurately weigh 1.0g each of 2 parts of Baiji powder (batch number: 20110702) (passed through a No. After cooling, make up the weight with a solvent, filter, discard the initial filtrate, take the subsequent filtrate, filter it with a 0.45 μm microporous membrane, and use it as the test solution.

[0044] Through the comparison of these two solvent extractions, the chromatographic peak information of the main components of the ethanol extract is smaller than that of the methanol extract, and the corr...

Embodiment 2

[0067] Embodiment 2: the determination of chromatographic analysis conditions

[0068] (1) Selection of mobile phase

[0069] Baiji contains complex components, and the polar range span is relatively large, it is difficult to separate isocratic elution, so the gradient elution method is used. Compare the elution effects of methanol-water, acetonitrile-water, acetonitrile-0.1% phosphoric acid water, acetonitrile-0.1% acetic acid water systems.

[0070] Select the elution program with better separation effect from the elution programs optimized during the experiment, and use methanol-water, acetonitrile-0.1% phosphoric acid water, acetonitrile-water, acetonitrile-0.1% acetic acid water as mobile phases respectively. As a result, the baseline of the spectrum measured by the acetonitrile-water system is relatively stable, and the main chromatographic peak information is more, so acetonitrile-water is finally selected as the mobile phase, and Table 1 is the elution procedure. Fi...

Embodiment 3

[0096] Example 3: Fingerprints of main components of Baiji decoction pieces

[0097] Referring to the "Technical Guidelines for Research on Fingerprints of Traditional Chinese Medicine Injections (Trial)", using the "Chinese Medicine Chromatographic Fingerprint Similarity Evaluation System Version A" software recommended by the Chinese Pharmacopoeia Commission, the similarity of the obtained fingerprints was compared (measured by median Establish a reference fingerprint), and conduct methodological investigation.

[0098] According to Embodiment 1 and 2, determine that the Baiji HPLC fingerprint is established as follows, (1) preparation of the test solution: accurately weigh the Baiji powder, pass No. 4 60-mesh sieve to obtain 1.0 g of Baiji powder, place Add 20mL of methanol to the Erlenmeyer flask with a stopper, weigh it, let it stand for 0min, and extract it by ultrasonic for 30min, the power of the ultrasonic wave is 280W, the frequency is 40kHz, let it cool, then weigh ...

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Abstract

The invention provides a method for establishing a rhizoma bletillae high performance liquid chromatography (HPLC) fingerprint spectrum, as well as a rhizoma bletillae standard fingerprint spectrum obtained by using the method. According to the scheme, the method comprises the following steps: (1) preparing a test solution; and (2) performing HPLC chromatographic analysis. The rhizoma bletillae HPLC standard fingerprint spectrum has 13 chromatographic peaks which have the respective retention time of 2.024 minutes, 5.928 minutes, 10.765 minutes, 16.133 minutes, 17.279 minutes, 20.999 minutes, 23.232 minutes, 24.678 minutes, 25.924 minutes, 28.287 minutes, 30.366 minutes, 32.529 minutes and 34.291 minutes. According to the method, the test solution is easy and convenient to prepare, the chromatographic conditions are easily realized, the method is high in stability and reproducibility, the quality of rhizoma bletillae can be effectively controlled, and the method provides reference for quality control of rhizoma bletillae.

Description

technical field [0001] The invention relates to a method for establishing fingerprints of traditional Chinese medicinal materials, in particular to a method for establishing fingerprints of baiji high performance liquid chromatography, and baiji standard fingerprints obtained by the method. The invention belongs to the technical field of pharmaceutical analysis. Background technique [0002] Baiji (Bletilla striata (Thunb.) Reichb.F.) is an orchid plant with dry tubers, slightly cold in nature, bitter, sweet, and astringent, and returns to the lung, stomach, and liver channels; Efficacy, used for hemoptysis, vomiting blood, traumatic bleeding, sore swelling, chapped skin. The quality control of the Chinese Pharmacopoeia 2010 edition is limited to the original plant species, medicinal properties and simple physical and chemical identification, lacking a set of effective internal quality control methods. Although there are successive literatures on the content determination ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N30/02G01N30/86
Inventor 陈蔚文严萍张蕾林文华张敏梁小银李璐詹若挺
Owner GUANGZHOU UNIVERSITY OF CHINESE MEDICINE
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