Method for determining effective component of total glycoside in smilax glabra ethanol water solution extract

A technology of ethanol aqueous solution and active ingredients, which is applied in the field of determination of total glycoside active ingredients in the ethanol aqueous extract of Smilax cocos, and achieves the effects of high precision, easy mastery, and simple method

Active Publication Date: 2010-06-16
GUANGZHOU BAIYUNSHAN JINGXIUTANG PHARM CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

For the quality control of the total glucosides of Smilax cocos, there is no literature report at present

Method used

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  • Method for determining effective component of total glycoside in smilax glabra ethanol water solution extract
  • Method for determining effective component of total glycoside in smilax glabra ethanol water solution extract
  • Method for determining effective component of total glycoside in smilax glabra ethanol water solution extract

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0030] The preparation of embodiment 1 Smilax cocos total glycosides

[0031] Press the method of embodiment 2 in the document disclosed by CN1772170A. Ten batches of total glucosides of Smilax cocos were prepared. The batch numbers are: batch S1, batch S2, batch S3, batch S4, batch S5, batch S6, batch S7, batch S8, batch S9, batch S10.

Embodiment 2

[0032] Example 2 Determination of effective chemical components in total glucosides of Smilax cocos by high performance liquid chromatography, and establishes a standard fingerprint with astilbin chromatographic peak as internal reference peak

[0033] 1 Instruments and reagents

[0034] 1.1 Instrument

[0035] 1.2 High performance liquid chromatography: Agilent1100 high performance liquid chromatography, diode array detector.

[0036] 1.3 Reagent

[0037] Reference substance astilbin, self-made, colorless needle-like crystals, mp182-186°C, a single spot on the thin-layer spectrum, HPLC detection as a single peak, the content of the area normalization method is greater than 99%. Methanol was chromatographically pure, and other reagents used were analytically pure.

[0038] 2 Methods and results

[0039] Chromatographic conditions: chromatographic column: octadecylsilane bonded silica gel column, model Lichrospher C-18 (4.6mm×250mm, 5μm); mobile phase: phase A is methanol, ...

Embodiment 3

[0047] Example 3 Determining the fingerprints of 10 batches of smilax glucosides, and determining the characteristic common peaks of smilax glucosides

[0048] Test method is the same as embodiment 2. The result is as image 3 shown.

[0049] The chromatographic peak of astilbin was used as the internal reference peak, and its retention time was 1 to calculate the relative retention time.

[0050] By measuring the fingerprints of 10 batches of smilax total glycosides and comparing their chromatograms, according to the relevant principles of the "Technical Requirements for Fingerprint Research of Traditional Chinese Medicine Injections" promulgated by the State Drug Administration, it is determined that there are 10 common peaks. The statistical results of the relative retention times of the common peaks of 10 batches of total glycosides are shown in Table 2. From the results in Table 2, the relative retention time RSDs of the 10 common peaks are all less than 3%, which is r...

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PUM

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Abstract

The invention relates to a method for determining an effective component of total glycoside in smilax glabra ethanol water solution extract and belongs to the field of pharmaceutical analysis methods. The method adopts a high-efficiency liquid chromatography to establish a fingerprint chromatogram characterized by taking the astilbin chromatographic peak as an internal reference peak, comprising the following steps of (a) putting 1g of smilax glabra total glycoside dry powder into a 25mL volumetric flask, adding methanol for dissolution and diluting the solution to a scale to obtain sample solution; (b) putting astilbin into methanol solution to prepare reference solution with the concentration of 0.1mg of astilbin per ml; (c) including chromatographic conditions: the chromatographic column is octadecylsilyl as filling; the mobile phase: A phase is methanol, and B phase is gradient elution formed by 0.3 percent of acetic acid solution; the flow velocity is 0.8ml/min; the detection wavelength is 323-327nm; the column temperature is 25-35 DEG C; and the theoretical plate number is over 3000 based on astilbin peak; and (d) determination. The method is simple, convenient and stable, has high precision, good reproducibility and easy control and can characterize the mass of the smilax glabra total glycoside.

Description

technical field [0001] The invention relates to the field of drug analysis methods, in particular to a method for determining the effective components of total glycosides in the ethanol aqueous extract of Smilax smilax. technical background [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, clinical application, etc., the varieties in the production and management of Smilax smilax are relatively chaotic. 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 lo...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): A61K36/896G01N30/36A61P13/00A61P15/00A61P17/00A61P31/00A61P33/14A61P39/02A61P29/00
Inventor 陈婷周翔徐强严志标陆颂规彭红英曾利杰
Owner GUANGZHOU BAIYUNSHAN JINGXIUTANG PHARM CO LTD
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