Anemone flaccida medicinal material HPLC-UV characteristic spectrum construction method

A technology of characteristic map and construction method, applied in the field of construction of characteristic map of traditional Chinese medicine Diwu, can solve the problems of research, lack of overall quality evaluation of Diwu medicinal materials, etc., and achieve the effect of simple operation and good repeatability

Active Publication Date: 2016-08-24
广州康和药业有限公司
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AI Technical Summary

Problems solved by technology

[0007] At present, the research on the quality standard of Diwu mainly focuses on the application of ultraviolet-visible spectrophotometry (UV-Vis) method to determine the content of total saponins (Wang Aimin, Chinese Pharmacy, 2007,18(21):1654-1655) and the application of HPLC Chromatographic (HPLC) method

Method used

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  • Anemone flaccida medicinal material HPLC-UV characteristic spectrum construction method
  • Anemone flaccida medicinal material HPLC-UV characteristic spectrum construction method
  • Anemone flaccida medicinal material HPLC-UV characteristic spectrum construction method

Examples

Experimental program
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Effect test

Embodiment 1

[0029] Example 1 Preparation, purification and structural identification of main chemical components in Diwu medicinal material

[0030] Such as figure 1 As shown, take 110g of total saponins of the root, dissolve it with 300mL of water, put the sample on the treated MCI small-pore resin column, and elute with water, 15%, 30%, 50%, 70% and 90% methanol successively, The 70% methanol eluted fraction was collected and concentrated to dryness under reduced pressure to obtain a dry extract (39.36 g). The extract was dissolved in 50% methanol, loaded on an ODS column, and eluted with a gradient of 60% to 95% methanol, and the eluted part of 60% methanol was separated by Sephadex LH-20 gel column chromatography and preparative HPLC [Cosmosil 5C 18 -MS-Ⅱ (20mm×250mm, 5μm) chromatographic column, the mobile phase is 30% acetonitrile-0.01% trifluoroacetic acid aqueous solution, the flow rate is 6.0mL min -1 ], to obtain compounds 2 (300mg) and 3 (200mg), 65% methanol elution site was...

Embodiment 2

[0071] Example 2 Construction method of characteristic map of Diwu medicinal material

[0072] (1) Preparation of reference substance solution

[0073] Accurately weigh an appropriate amount of each reference substance, add 30% acetonitrile to make anhuienoside E (0.25mg·mL -1 ), glycoside St-14a (0.25mg·mL -1 ), hemsgiganoside B (0.25mg·mL -1 ), flaccidoside II (0.5mg·mL -1 ), hederasaponin B (0.25mg·mL -1 ) of the reference substance solution, filtered, and obtained.

[0074] Table 3 Purity of reference substance

[0075]

[0076] Note: S is the reference peak

[0077] (2) preparation of need testing solution

[0078] Take about 0.5g of Diwu sample powder, weigh it accurately, put it in a stoppered Erlenmeyer flask, add 50mL of 75% methanol accurately, weigh it, extract it by ultrasonic, let it cool, make up the lost weight, shake well, and use 0.22μm Membrane filtration, take the continued filtrate, that is.

[0079] (3) Establishment of HPLC-UV chromatographic ...

Embodiment 3

[0092] Example 3 Determination Method of Characteristic Map of Diwu Medicinal Material

[0093] (1) Preparation of test solution

[0094] Take about 0.5g of Diwu medicinal material sample powder, accurately weigh it, put it in a stoppered Erlenmeyer flask, add 50mL of 75% methanol precisely, seal it tightly, weigh it, treat it ultrasonically for 40 minutes, let it cool, weigh it again, and use Make up the lost weight with 75% methanol, shake well, filter with a 0.22μm filter membrane, and take the subsequent filtrate to obtain the test solution.

[0095] (2) Determination by high performance liquid chromatography

[0096] The need testing solution of step (1) is carried out high performance liquid chromatography to measure, and chromatographic condition is:

[0097] Agilent 1260 high performance liquid chromatography; column: Cosmosil 5C 18 -MS-Ⅱ (4.6mm×250mm, 5μm); mobile phase: acetonitrile-0.01% trifluoroacetic acid solution (30:70); detection wavelength: 205nm; flow rat...

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Abstract

The invention belongs to the field of analysis and detection of traditional Chinese medicines and discloses an anemone flaccida medicinal material high performance liquid chromatography (HPLC) characteristic spectrum construction method for solving quality control problem of an anemone flaccida medicinal material. The method comprises the following steps: (1) preparing a reference solution; (2) preparing a test solution; (3) establishing chromatographic conditions; and (4) constructing characteristic spectrum. The method disclosed by the invention has the advantages of simple operation, accuracy, reliability and good repeatability, and multiple main effective ingredients in the anemone flaccida medicinal material can be more comprehensively detected, so that the anemone flaccida medicinal material HPLC-UV characteristic spectrum is constructed.

Description

technical field [0001] The invention relates to the field of quality control of traditional Chinese medicine, in particular to a method for constructing characteristic maps of traditional Chinese medicine Diwu. Background technique [0002] Quality control of traditional Chinese medicine refers to monitoring the quality of traditional Chinese medicine by adopting necessary analytical methods and detection means to ensure the safety, effectiveness, stability and controllability of traditional Chinese medicine. Due to the wide variety of Chinese herbal medicines and complex chemical composition, the development level of quality control of Chinese medicine has been unable to meet the development of modern Chinese medicine industry. The current quality control mode of traditional Chinese medicine is mostly established by referring to the quality control mode of foreign chemical drugs, and only one or several components are determined for content, which cannot reflect the complex...

Claims

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Application Information

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IPC IPC(8): G01N30/88
CPCG01N30/88G01N2030/8809
Inventor 范春林王英杨伟群叶文才裴红鲁展雨
Owner 广州康和药业有限公司
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