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4-H-Celastrus angulatus original medicine and preparation method and quality detection method thereof

A quality detection method, the technology of picroderm, applied in the field of botanical pesticides

Active Publication Date: 2014-07-30
河南省科高植物天然产物开发工程技术有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0008] In order to solve the problems existing in the prior art and quality of botanical pesticides, the object of the present invention is to provide a good botanical pesticide 4-H-pictericin and its aqueous emulsion

Method used

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  • 4-H-Celastrus angulatus original medicine and preparation method and quality detection method thereof
  • 4-H-Celastrus angulatus original medicine and preparation method and quality detection method thereof
  • 4-H-Celastrus angulatus original medicine and preparation method and quality detection method thereof

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Experimental program
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Effect test

preparation example Construction

[0123] iv) Preparation of test solution

[0124] Accurately weigh 200 mg of 4-H-piculin or 4-H-piculin aqueous emulsion in a 100mL volumetric flask, add appropriate amount of methanol to dissolve, dilute to the mark after ultrasonic oscillation, and shake well to obtain 4- H-picterine original medicine or 4-H-pichortine water emulsion for testing solution.

[0125] v) Precision determination

[0126] The test solution was injected three times, the relative standard deviation of the peak area was RSD=1.66%, and the relative standard deviation of the retention time was RSD=0.35%.

[0127] vi) Determination of the test product

[0128] Draw each test solution, inject sample, measure its peak area, obtain Angulateoid C content.

[0129] vii) Determination of recovery rate

[0130] Using the standard addition method, 100 μg / mL was added to the test sample 1, the average recovery rate was 102.3%, and the RSD was 2.12%.

[0131] ②Angulateoid C absolute content calculation

[01...

Embodiment 1

[0251] (1) The preparation method of 4-H-picterine original drug A

[0252] Add 3:3:3 times the volume of petroleum ether to the Hubei Enshi (2010) bitter vine seeds (24 mesh) that meet the requirements after sieving, and reflux extraction at 80°C for 3 times, each time for 2 hours , filtered, combined three filtrates, and concentrated under reduced pressure to seed oil. Take this oil, pack it into a column (diameter-to-height ratio: 10:1) with its weight of 1 times the amount of HP20 resin, and successively wash the column with 40% ethanol, 60% ethanol, 80% ethanol and 95% ethanol (the The volume of ethanol was 40, 90, 40 and 20 times that of the filtrate after concentration), and the 60% ethanol eluate was collected and evaporated to dryness under reduced pressure to obtain the original drug A of 4-H-pichoretine.

[0253]

[0254] (2) Quality testing method of 4-H-picterine original drug A

[0255] ①Preparation of characteristic extracts

[0256] Take 4-H-picterine ori...

Embodiment 2

[0269] (1) The preparation method of the original drug B of 4-H-piculin

[0270] After sieving, the seeds (24 mesh) of Phyllostachys chinensis (2011) that met the requirements were added to ethanol with a volume of 3︰2︰2 times and a mass ratio of 95%, and reflux extraction at 60°C for 3 times. Extract each time for 1.5h, filter, combine three filtrates, and concentrate under reduced pressure to seed oil. Take this kind of oil, use its weight as 1.2 times the amount of D-101 resin to pack into a column (diameter-to-height ratio 10:1), and successively wash the column with 35% ethanol, 65% ethanol, 80% ethanol and 90% ethanol (punch column 40, 90, 40 and 20 times the volume of the ethanol after concentrating the filtrate respectively), collect the 65% ethanol eluate, and evaporate to dryness under reduced pressure to obtain the original drug B of 4-H-pichoretine.

[0271]

[0272] (2) 4-H-Pictericillin Technical B quality testing method

[0273] ①Preparation of characterist...

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Abstract

The invention relates to a 4-H-Celastrus angulatus original medicine and an emulsion in water thereof as well as a preparation method and a quality detection method thereof. The 4-H-Celastrus angulatus original medicine comprises the active components in percentage by weight as follows: 15.0-18.0% of Angulateoid C, 4.0-12.0% of Angulateoid B, 13.0-21.0% of Angulateoid E, 4.5-8.0% of Angulatinoid I, 4.5-7.0% of Angulatinoid V, 3.0-5.0% of Angulatinoid II, 2.0-6.0% of Celahin B and 2.0-6.0% of Celahin C. The 4-H-Celastrus angulatus original medicine is prepared by a macroreticular resin method. The quality detection method adopts IGD (Immunoglobulin) nuclear magnetic resonance carbon spectrum coupling fingerprint technology. The content of the 4-H-Celastrus angulatus original medicine is greatly improved, and the quality detection method is higher in accuracy, stability, repeatability and accessibility.

Description

technical field [0001] The invention belongs to the technical field of botanical pesticides, in particular, it relates to a 4-H-picterine original drug and its water emulsion, as well as their preparation method and quality detection method. Background technique [0002] Celastrus angulatus MaXim is a perennial vine-like shrub of Celastraceae (Celastraceae), distributed in Hebei, Shandong, Henan, Shaanxi, Hubei, Gansu, Jiangsu, Anhui and other provinces [Chinese Academy of Sciences Flora of China Editorial Committee. Flora of China. Science Press, 1999,45(3):102]. Phyllostachys chinensis is a unique insecticidal plant in my country. It has multiple functions, has different physiological activities against different pests, has stable performance, is safe to use, does not kill natural enemies, and is non-polluting. At present, the vast majority of products related to Phyllostachys chinensis use the root / bark [CN92113104.6; CN94103655.3; CN99109275.9; CN02122988.0], and the sc...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): A01N43/40A01N43/12A01N25/04A01P7/04G01N24/08G01N30/02
Inventor 赵天增张海艳董建军魏悦于立芹范毅常霞郭唯景炳年刘雨晴李自红
Owner 河南省科高植物天然产物开发工程技术有限公司
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