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Celangulin mother liquor and preparation method and quality inspection method thereof

A quality detection method and a technology for picrophyllin, which are applied in the field of botanical pesticides and can solve problems such as unreported

Active Publication Date: 2013-02-06
河南省科高植物天然产物开发工程技术有限公司 +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

At present, there is no report on the fingerprints of the mother liquor of picroderm and its emulsion in water

Method used

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  • Celangulin mother liquor and preparation method and quality inspection method thereof
  • Celangulin mother liquor and preparation method and quality inspection method thereof
  • Celangulin mother liquor and preparation method and quality inspection method thereof

Examples

Experimental program
Comparison scheme
Effect test

preparation example Construction

[0107] 1. Preparation method of 10% celangulin mother liquor and water emulsion

[0108] (1) 10% Celangulin mother liquor

[0109] Weigh the dried bitter vine root or / and bark, smash it through a 10~24 mesh sieve, and use 5~7 times the volume of benzene to extract 1~2 times at 45~55℃ by ultrasonic circulation, each extraction 35~ For 55 minutes, the filtrates are combined and concentrated under reduced pressure to an extract with a density of about 1.1 to 1.3, and a 10% celangulin mother liquor is obtained.

[0110] (2) 2% celangulin water emulsion

[0111] After 10% celangulin mother liquor and emulsifier are stirred and mixed in a certain proportion, a certain proportion of antifreeze is added and the balance is made up with water. After shearing and homogenization, 2% celangulin aqueous emulsion is obtained.

[0112] The mixing ratio of 2% celangulin water emulsion is as follows:

[0113] 10% celangulin mother liquor 15-20%, emulsifier 8-12%, antifreeze 3-4%, water makes up the balan...

Embodiment 1

[0272] Example 1: Preparation and control effect of 10% celangulin mother liquor and 2% celangulin aqueous emulsion

[0273] (1) Preparation of 10% celangulin mother liquor

[0274] After sieving, the root and bark of the vine root and bark that meet the requirements (24 mesh) are 5-7 times the volume of benzene (raw material: benzene = kg: L, that is, 1kg of vine root and bark uses 5-7L of benzene ) 50℃ ultrasonic cycle extraction 35~55min (ultrasonic power 500W) 1~2 times (the extraction conditions are the same each time), the filtrate is combined and concentrated into 1.1~1.3 extract under reduced pressure, and then 10% celangulin mother liquor is obtained . See the table below for specific data.

[0275]

[0276] (2) Preparation of 2% celangulin water emulsion

[0277] Place the qualified 10% celangulin mother liquor in the reaction kettle, add the auxiliary materials (emulsifier and antifreeze) in the following table according to the proportion, stir, then add the solvent to th...

Embodiment 2

[0300] Example 2: 10% celangulin mother liquor (Xichuan, Henan) IGD nuclear magnetic resonance carbon spectroscopy coupled fingerprint spectrum quality detection method

[0301] (1) Preparation of characteristic extracts of mother liquor

[0302] Choose 10% celangulin mother liquor (Xichuan, Henan), and prepare the characteristic extract of 10% celangulin mother liquor according to the following method: Weigh 20g of 10% celangulin mother liquor, filter and concentrate under reduced pressure at 60℃, Recover the solvent to the form of extract. After the extract is dissolved with 6 times the volume (120mL) and 80% mass ratio of methanol, 3 times the volume (60mL) of petroleum ether is extracted once, each extraction is 30min, and the methanol layer is filtered. After concentration under reduced pressure, the solvent was recovered to dryness, and the characteristic extract of 10% celangulin mother liquor (Xichuan, Henan) was obtained.

[0303] (2) IGD nuclear magnetic resonance carbon s...

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Abstract

The invention relates to celangulin mother liquor and emulsion in water, a preparation method and a quality inspection method thereof. The celangulin mother liquor comprises, by mass, active ingredients of 1.9-3.5% of angulatin A, 3.0-5.0% of angulatin B, 2.5-4.0% of angulatin G and 2.50-4.10% of angulatin E. The celangulin mother liquor is prepared by an ultrasonic recycling extraction method, and the quality inspection method adopts the IGD carbon-13 nuclear magnetic resonance spectroscopy coupling fingerprint technology. The celangulin mother liquor content is increased greatly, and accuracy, stability, repeatability and feasibility of the quality inspection method are high.

Description

Technical field [0001] The invention belongs to the technical field of plant-derived pesticides, and specifically relates to a mother liquor of celangulin and its water emulsion, as well as their preparation method and quality detection method. Background technique [0002] Plant-derived pesticides belong to a branch of the category of biological pesticides, which use certain types of stable ingredients contained in plants as active ingredients to implement insecticidal and sterilization effects. Because these active ingredients are derived from plants themselves, they are easy to decompose naturally; and because of their structural diversity, it is difficult for harmful organisms to develop resistance. Therefore, plant-derived pesticides are one of the main directions for the development of green pesticides in the world in the future. Domestic botanical pesticides include pyrethrum, neem, matrine, nicotinic insecticides, and celangulin insecticides, etc. [①Wei Yanmin. Questions...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): A01N43/12A01N25/04A01P7/04A01P7/02G01N24/08G01N30/02
Inventor 赵天增张海艳董建军范毅于立芹魏悦刘雨晴郭唯常霞陈玲李倩
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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