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Production method of spinosin

A production method and technology for extracting liquid, which are applied in the production field of spinosin, can solve the problems of small preparation amount, unsuitable for industrial production and the like, and achieve the effects of short production cycle, low cost and high product safety.

Inactive Publication Date: 2012-07-25
苏州宝泽堂医药科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Li Huijun and Li Ping used high performance liquid chromatography to simultaneously determine the content of spinosin and 6'"-feruloylspinosin, and prepared by degreasing petroleum ether, refluxing methanol, separating on silica gel column, and eluting with chloroform-methanol For the test solution, this method uses a large amount of harmful reagents such as chloroform and methanol, and the preparation amount is small, so it is not suitable for industrial production

Method used

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  • Production method of spinosin

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Effect test

Embodiment 1

[0031] Crumble jujube kernels into coarse powder, take 1kg and put it in a 10L extraction tank, add 6L of 80-100℃ hot water to decoct and extract, extract twice, each time for 2 hours, filter, combine the two extracts, and put the extract on S -8 macroporous adsorption resin column, first eluted with 3000ml of cold water, then eluted with 6000ml of 60% ethanol, collected the 60% ethanol eluate, added 200g of diatomaceous earth to stir and decolorize, filtered, and concentrated the decolorized solution to obtain a concentrated solution; Put the concentrated solution on a polyamide column, elute with 1000ml30% ethanol first, then elute with 1250ml75% ethanol, collect the 75% ethanol eluate, recover ethanol under reduced pressure, concentrate to obtain spinosin coarse crystals, and use the crude crystals The acetone was heated to reflux to dissolve, cooled to room temperature, left to stand for crystallization, the crystals were filtered out, and vacuum-dried to obtain 853 mg of h...

Embodiment 2

[0033] Crumble jujube kernels into coarse powder, take 1kg and put it in a 10L extraction tank, add 20L of 60-80°C hot water for constant temperature soaking and extraction, extract 3 times, 2 hours each time, filter, combine the three extracts, put the extract on AB- 8 macroporous adsorption resin columns, first elute with 4L of cold water, then elute with 12L of 80% ethanol, collect the 80% ethanol eluate, add 500g of diatomaceous earth to stir for decolorization, filter, and concentrate the decolorization solution to obtain a concentrated solution; Put the concentrated solution on a polyamide column, first elute with 1200ml of 20% acetone, then elute with 1500ml of 80% acetone, collect the 80% acetone eluate, recover the acetone under reduced pressure, concentrate to obtain spinosin coarse crystals, and use acetone to wash the coarse crystals Heated to reflux to dissolve, cooled to room temperature, left to stand for crystallization, filtered out the crystals, and vacuum dri...

Embodiment 3

[0035] Crumble jujube kernels into coarse powder, take 2kg and put it in a 20L extraction tank, add 16L of 70-90℃ hot water for ultrasonic extraction, extract 3 times, each time for 0.5 hours, filter, combine the three extracts, and put the extract on X-3 Macroporous adsorption resin column, first elute with 10L of cold water, then elute with 15L of 75% ethanol, collect the 75% ethanol eluate, add 750g of diatomaceous earth to stir for decolorization, filter, and concentrate the decolorization solution to obtain a concentrated solution: concentrate Put the liquid on a polyamide column, first elute with 2L of 20% ethanol, then elute with 3L of 90% ethanol, collect the 90% ethanol eluate, recover ethanol under reduced pressure, concentrate to obtain spinosin coarse crystals, and heat the coarse crystals with acetone Reflux to dissolve, cool to room temperature, stand still for crystallization, filter out the crystals, and dry in vacuum to obtain 1.67 g of high-purity spinosin fin...

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Abstract

The invention discloses a production method of spinosin, which comprises the following steps: breaking wild jujube seeds, extracting by hot water and extracting to obtain extracted liquid; making the extracted liquid pass through a macroporous resin column for chromatography; collecting the extracted liquid which enriches the target element; adding 4-6% diatomite for decolorization; concentrating the decolorized liquid to obtain crude extract; making the crude extract pass through a polyamide resin column for chromatography; eluting by low-carbon alcohol or low-carbon ketone solution with different concentrations to elute in turns; collecting the eluted solution, concentrating to obtain crude spinosin crystals; and performing reflux and dissolution to the crude spinosin crystals by acetone, cooling and crystallizing, filtering and drying to obtain the finished product. The invented production method uses the hot water to replace organic solvent to perform the extraction, uses the macroporous resin column to replace a silica gel column to perform the chromatography, and uses the low-carbon alcohol and the low-carbon ketone to replace poisonous solvent chloroform; the cost is reduced, the production safety is good, and the product purity is high.

Description

Technical field: [0001] The invention belongs to the field of traditional Chinese medicine chemistry, and in particular relates to a production method of spinosin. Background technique: [0002] Ziziphus jujube kernel, also known as white spines, spiny needles, jujube kernels, and wild jujube seeds, is the dry mature seed of Ziziphus jujube Mill.var.spinosa (Bunge) Hu ex H.F.Chou, a plant of Rhamnaceae. Sweet, sour, flat, return liver, gallbladder, heart meridian. It has the effects of nourishing the heart and nourishing the liver, calming the mind and calming the nerves, suppressing sweat, and promoting body fluid. It is used for insomnia, palpitations and dreaminess, body deficiency and hyperhidrosis, and thirsty wounds. Suanzaoren was first recorded in "Shen Nong's Materia Medica", and is mainly produced in Hebei, Shaanxi, Liaoning, and Henan. Its chemical composition mainly contains fatty acids, triterpene saponins, flavonoids, steroids and alkaloids. Among them, the ...

Claims

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Application Information

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IPC IPC(8): C07H17/07C07H1/08
Inventor 李法庆刘东锋
Owner 苏州宝泽堂医药科技有限公司
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