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Method for detecting active ingredients in American cockroach extract

A technology of Periplaneta americana and active ingredients, applied in the field of detection of active ingredients in the extract of Periplaneta americana, can solve the problems of low content, existing difficulties, difficult implementation of conventional detection methods, etc.

Inactive Publication Date: 2011-01-26
ZHEJIANG JINGXIN PHARMA +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The quality control detection method of KFX-4 in Kangfuxin liquid has not been reported in the literature, and because of its low content, the interference of impurities is very serious, and the conventional detection method is difficult to implement and there are difficulties

Method used

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  • Method for detecting active ingredients in American cockroach extract
  • Method for detecting active ingredients in American cockroach extract
  • Method for detecting active ingredients in American cockroach extract

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0024] Preparation of Periplaneta americana extract: (the following batches of Periplaneta americana extracts used for detection are all prepared according to this method)

[0025] Get dry Periplaneta americana 1kg, put in the extraction pot, add 90% ethanol solution, soak three times at 60 ℃, each 12 hours, the first time with ethanol is eight times the amount of Periplaneta americana; Six times the amount; the third four times the amount. Combine warm infusions, filter and concentrate, and recover ethanol until there is no alcohol smell. The resulting concentrated solution plus purified water is 1-2 times the amount of Periplaneta americana. Stand still for more than 24 hours, separate and discard the precipitate and oil layer, filter the aqueous solution, and concentrate under reduced pressure to a relative density of 1.15-1.20 (70°C).

Embodiment 2

[0027] Take 1g of Periplaneta americana extract with batch number T09070101, weigh it accurately, put it in a 10ml measuring bottle, add about 5-7ml of water, dissolve it by ultrasonic, and dilute to 10ml. Centrifuge, take 1ml of supernatant, pass through Strata X solid-phase extraction column, wash twice with water, 2ml each time, discard, use 20% methanol, 30% methanol, 50% methanol each 2ml for elution in sequence, combined elution solution, placed in a water bath and evaporated to dryness, the residue was dissolved in 50% methanol and quantitatively transferred to a 1ml or 2ml measuring bottle, centrifuged, and the supernatant was taken for chromatographic analysis [chromatographic analysis conditions: octadecylsilane bonded silica gel as filler; Using methanol-water (20:80) V / V as the mobile phase, the flow rate is 0.8ml / min; the detection wavelength is 265nm, the injection volume is 5μl, and the content of KFX-4 is calculated by the peak area external standard method]. A...

Embodiment 3

[0029] Take about 1 g of Periplaneta americana extract from batch number T09070101, weigh it accurately, put it in a 10 ml measuring bottle, add about 5-7 ml of water, heat or sonicate to dissolve, and constant volume. Centrifuge, take 1ml of supernatant, pass through ODS (octadecylsilane bonded silica gel) solid-phase extraction small column, wash twice with water, 2ml each time, discard, use 20% methanol, 30% methanol, 50% methanol Each 2ml was eluted successively, and the combined eluents were evaporated to dryness in a water bath. The residue was dissolved in 50% methanol and quantitatively transferred to a 1ml or 2ml measuring bottle, centrifuged, and the supernatant was taken for chromatographic analysis (method is the same as in Example 1). As a result, the content of KFX-4 was determined to be 0.483mg / g.

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Abstract

The invention provides a method for detecting an active ingredient (3R) -3-methyl-7-hydroxymethyl-8-hydroxyl-3,4-dihydroisocoumarin-6-O-beta-D-glucopyranoside, namely KFX-4 in an American cockroach extract. In the method, high performance liquid chromatography (HPLC) is adopted, octadecylsilane chemically bonded silica is taken as a filler; methanol or acetonitrile-water (0-50:100-50 V / V) is taken as a mobile phase of which the flow speed is between 0.2 and 2.0 ml / min; the detection wavelength is one or more wavelengths of between 210 and 400 nanometers; a diode array detector is adopted; the sample size is between 5 and 50 mu l; theoretical plate number is not less than 4,000 when calculated according to a KFX-4 peak; the separation degree with a neighboring impurity peak is more than 1.5; chromatographic analysis is performed; and KFX-4 content is calculated by a peak area external standard method. An effective quality control method is provided for Chinese medicinal Kangfuxin solution and the method has a large practical value in the aspect of improving product quality and medicament safety.

Description

technical field [0001] The invention relates to a drug detection method, in particular to a detection method of the main active ingredient of the Chinese medicine Kangfuxin Liquid, an extract of the American cockroach, and in particular to a detection method of the active ingredient in the American cockroach extract. Background technique [0002] The traditional Chinese medicine Kangfuxin Liquid is a product that the applicant has been on the market for many years, and its main component is the extract of Periplaneta americana. Function cures mainly: tonifying blood vessels, nourishing yin and promoting muscle growth. Oral administration: for blood stasis and yin stagnation, stomach pain and bleeding, gastric and duodenal ulcers; and adjuvant treatment of yin deficiency pulmonary tuberculosis and tuberculosis. It is externally used on wounds of gold sores, trauma, ulcer burns, and decubitus sores. [0003] There are few reports on the medicinal active ingredients in Peripl...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N30/02G01N30/06
Inventor 陈鉴东余国珍
Owner ZHEJIANG JINGXIN PHARMA
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