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Method for determining active ingredients of rhizoma smilacis glabrae medicinal material

An effective ingredient, a technology for Poria cocos, which is applied in the field of establishing a fingerprint spectrum for determining the active ingredients of Poria cocos, can solve the problems that the quality control of the medicinal materials cannot be met, the quality of the traditional Chinese medicinal materials cannot be effectively controlled, etc., and the method is easy to master and simple. , the effect of accurate authenticity

Active Publication Date: 2010-06-02
GUANGZHOU BAIYUNSHAN JINGXIUTANG PHARM CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The analysis method in the Pharmacopoeia Consultation Draft only conducts qualitative and quantitative analysis of a certain active ingredient of Chinese medicinal materials, and cannot effectively control the quality of Chinese medicinal materials, so it cannot meet the needs of quality control of medicinal materials in production

Method used

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  • Method for determining active ingredients of rhizoma smilacis glabrae medicinal material
  • Method for determining active ingredients of rhizoma smilacis glabrae medicinal material
  • Method for determining active ingredients of rhizoma smilacis glabrae medicinal material

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0033] Example 1 High-performance liquid chromatography was used to determine the effective components of the medicinal material Smilax smilax, and to establish a standard fingerprint with the astilbin chromatographic peak as the internal reference peak

[0034] 1 Instruments and reagents

[0035] 1.1 Instrument

[0036] High performance liquid chromatography: Agilent1100 high performance liquid chromatography, diode array detector.

[0037] 1.2 Reagent

[0038] Reference substance astilbin, self-made, colorless needle-like crystals, mp 182-186°C, a single spot on the thin-layer spectrum, HPLC detection is basically a single peak (such as figure 1 Shown), the area normalization method assay content is greater than 99%. Smilax smilax medicinal materials are purchased in medicinal materials market.

[0039] 2 Methods and Results

[0040] Chromatographic conditions: chromatographic column: octadecylsilane bonded silica gel column, model Lichrospher C-18 (4.6mm×250mm, 5μm); ...

Embodiment 2

[0048] Example 2 Measure the fingerprints of 10 batches of Smilax smilax medicinal materials, and determine the characteristic common peaks of Smilax smilax medicinal materials

[0049] Test method is the same as embodiment 1. The result is as image 3 shown. Ten batches of medicinal materials were purchased from Guangxi (batch numbers S1, S2, S3, S4), Hunan (batch numbers S5, S6, S7), and Zhejiang (batch numbers S8, S9, S10).

[0050] The statistical results of the relative retention time of the common peaks of the above 10 batches of medicinal materials are shown in Table 2. From the results in Table 2, the relative standard deviations (abbreviated as RSD, hereinafter the same) of the relative retention times (abbreviated RT, hereinafter the same) of the 12 common peaks are all less than 2%, relatively stable.

[0051]

[0052] By measuring the fingerprints of 10 batches of Smilax smilax medicinal materials and comparing their chromatograms, it is determined that there...

Embodiment 3

[0068] The precision test of embodiment 3 method of the present invention:

[0069] Taking Smilax smilax S2 batch as the test sample, take the same test sample solution, repeat the sample injection 6 times under the above-mentioned chromatographic conditions, record the retention time and peak area of ​​each characteristic peak, take astilbin as a reference, calculate each Relative retention times and peak areas of characteristic peaks. The results show that the RSD of the relative retention time of each common peak is not more than 1.0%, and the RSD of the relative peak area is not more than 1.5%. The results are shown in Table 4 and Table 5.

[0070] Table 4 precision test common peak relative retention time statistics

[0071]

[0072] Table 5 Precision test common peak relative peak area statistics

[0073]

[0074] Fingerprint reproducibility test:

[0075] Accurately weigh 6 parts of dried Smilax smilax medicinal material S2 powder, each part 1.0g, prepare the ...

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Abstract

The invention discloses a method for determining active ingredients of a rhizoma smilacis glabrae medicinal material, relating to the filed of medicament analysis. In the invention, a fingerprint taking an astilbin chromatographic peak as an internal reference peak is established. The method comprises the following steps of: (a) preparing a test article solution; (b) taking astilbin as a reference substance and taking 0.10mg / mL astilbin solution prepared from methanol as a reference substance solution; (c) chromatographic conditions: taking a chromatographic column made of octadecylsilane chemically bonded silica as filler; adopting gradient elution, detecting the wavelength of 325+ / -2 nm and the column temperature of 30+ / -5DEG C; calculating the theoretical column plate number not less than 3,000 according to astilbin peak; and (d) determining. The fingerprint established by rhizoma smilacis glabrae ethanol-soluble extractives contains active ingredients with main activity of rhizoma smilacis glabrae. The fingerprint is used for judging the quality of rhizoma smilacis glabrae and the one sidedness for judging the quality of rhizoma smilacis glabrae by determining one or two chemical components can be avoided. The method has the advantages of simpleness, convenience, stability, high precision, favorable reproduction, easy grasp and capability of rapidly and accurately identifying the authenticity and merits of products.

Description

Technical field [0001] The invention relates to the field of drug analysis, in particular to establishing a fingerprint method for determining effective components of Smilax smilax. Background technique [0002] Smilax smilax is the dry rhizome of Smilax glabra Roxb., a plant of Liliaceae; it has the functions of dehumidification, detoxification, and tonic joints. It is used for limb spasms and muscle and bone pain caused by damp-heat stranguria, vaginal discharge, carbuncle, scrofula, scabies, syphilis and mercury poisoning. Since the identification of varieties is not paid much attention to in the links of harvesting, circulation, and clinical application, the varieties in the production and operation of Smilax smilax are relatively chaotic and the quality varies greatly. For example: Smilax genus Smilax S.china L. is a confusing product. S. glauco-china Warb. is used as red soil ling in Nanchuan, Sichuan, and "fresh smilax" in Zhenjiang, Jiangsu, which is a local custom...

Claims

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Application Information

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IPC IPC(8): A61K36/896G01N30/02A61P29/00A61P15/00A61P31/06A61P17/00A61P19/00A61P19/08
Inventor 陈婷周翔徐强严志标曾利杰陆颂规彭红英
Owner GUANGZHOU BAIYUNSHAN JINGXIUTANG PHARM CO LTD
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