CN105669801A - Extraction technology for baicalin crude product - Google Patents

Extraction technology for baicalin crude product Download PDF

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Publication number
CN105669801A
CN105669801A CN201610125088.9A CN201610125088A CN105669801A CN 105669801 A CN105669801 A CN 105669801A CN 201610125088 A CN201610125088 A CN 201610125088A CN 105669801 A CN105669801 A CN 105669801A
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China
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baicalin
extraction
decoction pieces
skullcap root
baikal skullcap
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CN201610125088.9A
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Chinese (zh)
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霍应怀
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Individual
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    • CCHEMISTRY; METALLURGY
    • C07ORGANIC CHEMISTRY
    • C07HSUGARS; DERIVATIVES THEREOF; NUCLEOSIDES; NUCLEOTIDES; NUCLEIC ACIDS
    • C07H1/00Processes for the preparation of sugar derivatives
    • C07H1/06Separation; Purification
    • CCHEMISTRY; METALLURGY
    • C07ORGANIC CHEMISTRY
    • C07HSUGARS; DERIVATIVES THEREOF; NUCLEOSIDES; NUCLEOTIDES; NUCLEIC ACIDS
    • C07H17/00Compounds containing heterocyclic radicals directly attached to hetero atoms of saccharide radicals
    • C07H17/04Heterocyclic radicals containing only oxygen as ring hetero atoms
    • C07H17/06Benzopyran radicals
    • C07H17/065Benzo[b]pyrans
    • C07H17/07Benzo[b]pyran-4-ones

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  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Health & Medical Sciences (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Biochemistry (AREA)
  • Biotechnology (AREA)
  • General Health & Medical Sciences (AREA)
  • Genetics & Genomics (AREA)
  • Molecular Biology (AREA)
  • Medicines Containing Plant Substances (AREA)
  • Pharmaceuticals Containing Other Organic And Inorganic Compounds (AREA)

Abstract

The invention discloses an extraction technology for a baicalin crude product and belongs to the technical field of extraction of traditional Chinese medicine effective ingredients. The extraction technology for the baicalin crude product comprises the following steps: firstly carrying out ultraviolet radiation on scutellaria baicalensis decoction pieces, and then carrying out high pressure treatment, so that the baicalin crude product extraction efficiency is improved; and meanwhile, the extraction technology is simple, extraction cost is relatively low, thereby being applicable to large-scale popularization and application.

Description

A kind of crude baicalin extraction process
Technical field
The present invention relates to the extractive technique field of Effective Component of Chinese Medicine, specifically a kind of crude baicalin extraction process.
Background technology
Radix Scutellariae (ScutellariabaicalensisG) is conventional Chinese medicine. Commodity are mainly the root of China's the north labiate Radix Scutellariae; In addition, Scutellaria still has the root of several plant also to do Radix Scutellariae use in some area. Radix Scutellariae is mainly used in the effect such as antibacterial, antiinflammatory and immunomodulating, antipyretic-antalgic, Adjust-blood lipid and anti-AIDS. According to the literature, the effective ingredient of Radix Scutellariae is the flavone compounds such as baicalin, wogonoside and aglycon thereof.
Baicalin is content high (7.0-20%) in Radix Scutellariae, traditional baicalin preparation technology includes: methanol or ethanol extraction, concentration, plate-and-frame filtration method, acid is heavy and the step such as recrystallization, it also exists following deficiency: 1. contaminated environment: need to use the organic solvents such as substantial amounts of methanol in preparation process, big for environment pollution, poor stability; 2. industrial production cost is too high: existing technological operation complex steps, complexity, and heating and refluxing extraction needs to extract three times, and each 2h at least needs six hours, and the production cycle is long, and product loss is big, and finished product content of baicalin can only achieve 80%.
Summary of the invention
In order to avoid the deficiencies in the prior art, it is an object of the invention to provide a kind of crude baicalin extraction process.
In order to realize the purpose of the present invention, technical scheme provided by the invention is as follows:
A kind of crude baicalin extraction process, comprises the following steps:
(1) take baikal skullcap root decoction pieces, evenly laid out under uviol lamp, ultraviolet radiation 30-45min;
(2) it is 3-5h under 120KPa to 150KPa environment that the baikal skullcap root decoction pieces that (1) step has processed is placed in air pressure;
(3) by the baikal skullcap root decoction pieces after step (2) HIGH PRESSURE TREATMENT, the boiling water of 1.5-2 times of addition Radix Scutellariae weight, boil and carry 2-3 time, each 45min, filters, united extraction liquid, then extracting solution hydrochloric acid adjusts pH value to 1.5, precipitates out baicalin precipitation, rinses baicalin 3 times with circulating water, then, under 40-50 DEG C of condition, dry gained material is defined as crude baicalin in the present invention.
The beneficial effects of the present invention is: after Radix Scutellariae of the present invention carries out ultra-vioket radiation and HIGH PRESSURE TREATMENT before extracting, crude baicalin extraction efficiency increases, and extraction process of the present invention is simple, extraction cost is relatively low, it is adaptable to large-scale promotion uses.
Detailed description of the invention
Embodiment 1
A kind of crude baicalin extraction process, comprises the following steps:
(1) take baikal skullcap root decoction pieces 100g, evenly laid out under uviol lamp, ultraviolet radiation 30min;
(2) it is 3h under 120KPa environment that the baikal skullcap root decoction pieces that (1) step has processed is placed in air pressure;
(3) by the baikal skullcap root decoction pieces after step (2) HIGH PRESSURE TREATMENT, the boiling water of the 1.5 of addition Radix Scutellariae weight, boil and carry 2 times, each 45min, filters, united extraction liquid, then extracting solution hydrochloric acid adjusts pH value to 1.5, precipitates out baicalin precipitation, rinses baicalin 3 times with circulating water, then, under 40 DEG C of conditions, dry gained material is defined as crude baicalin in the present invention.
HIGH PRESSURE TREATMENT concrete operations are: the baikal skullcap root decoction pieces after ultraviolet is processed loads in stainless steel cask, uses air compressor, squeezes into air, and the air pressure squeezing into stainless steel cask controls at 120KPa.
Crude baicalin extraction process effect measuring of the present invention is tested
1st group, only by the step in embodiment 1 (1) in ultra violet lamp 30min, become infrared lamp irradiate 30min, all the other process steps all with embodiment 1 step (2), step (3) consistent.
2nd group, only by the step in embodiment 1 (1) in ultra violet lamp 30min, become daylight lamp irradiate 30min, all the other process steps all with embodiment 1 step (2), step (3) consistent.
3rd group, only by the step in embodiment 1 (1) in ultra violet lamp 30min, become electric filament lamp irradiate 30min, all the other process steps all with embodiment 1 step (2), step (3) consistent.
4th group, only by the step in embodiment 1 (1) in ultra violet lamp 30min, become electricity-saving lamp irradiate 30min, all the other process steps all with embodiment 1 step (2), step (3) consistent.
5th group, only by the step in embodiment 1 (1) in ultra violet lamp 30min, become electricity-saving lamp irradiate 30min, all the other process steps all with embodiment 1 step (2), step (3) consistent.
6th group, only by the step in embodiment 1 (1) in ultra violet lamp 30min, become light emitting diode irradiate 30min, all the other process steps all with embodiment 1 step (2), step (3) consistent.
7th group, only by the step in embodiment 1 (2) in process baikal skullcap root decoction pieces air pressure be 120KPa, become 119KPa air pressure, all the other process steps all with embodiment 1 step (1), step (3) consistent.
8th group, only by the step in embodiment 1 (2) in process baikal skullcap root decoction pieces air pressure be 120KPa, become 151KPa, all the other process steps all with embodiment 1 step (1), step (3) consistent.
To often organize after crude baicalin extracts according to the high-efficient liquid phase technique under 2010 editions Radix Scutellariae items of Chinese Pharmacopoeia, measure the amount of crude baicalin in radix scutellariae medicinal materials and extraction ratio.
Measurement result is as shown in table 1 below
Table 1 processing method is on the impact of crude baicalin content in baikal skullcap root decoction pieces
Group Crude baicalin amount (g) Extraction ratio %
1st group 45.8 45.8
2nd group 45.3 45.3
3rd group 45.9 45.9
4th group 44.9 44.9
5th group 48.2 48.2
6th group 47.6 47.6
7th group 43.4 43.4
8th group 45.2 45.2
Embodiment 1 65.8 65.8
As shown in Table 1, adopting the extraction process of the embodiment of the present invention 1, compared with 8 groups of extraction processes of the in table the 1st group of-, the extraction process of the application present invention, the amount of crude baicalin is greatly improved, and extraction efficiency increases, and therefore, is worth large-scale promotion application.
Embodiment 2
A kind of crude baicalin extraction process, comprises the following steps:
(1) take baikal skullcap root decoction pieces 150g, evenly laid out under uviol lamp, ultraviolet radiation 40min;
(2) it is 4h under 130KPa environment that the baikal skullcap root decoction pieces that (1) step has processed is placed in air pressure;
(3) by the baikal skullcap root decoction pieces after step (2) HIGH PRESSURE TREATMENT, the boiling water of 2 times of addition Radix Scutellariae weight, boil and carry 3 times, each 45min, filter, united extraction liquid, then extracting solution hydrochloric acid adjusts pH value to 1.5, precipitation baicalin precipitates, and rinses baicalin 3 times with circulating water, then under 50 DEG C of conditions, dry gained material is defined as crude baicalin in the present invention, according to the high-efficient liquid phase technique under 2010 editions Radix Scutellariae items of Chinese Pharmacopoeia, the amount of crude baicalin in radix scutellariae medicinal materials that measures is 100.3g, and extraction ratio is 66.9%.
HIGH PRESSURE TREATMENT concrete operations are: the baikal skullcap root decoction pieces after ultraviolet is processed loads in stainless steel cask, uses air compressor, squeezes into air, and the air pressure squeezing into stainless steel cask controls at 130KPa.
Embodiment 3
A kind of crude baicalin extraction process, comprises the following steps:
(1) take baikal skullcap root decoction pieces 200g, evenly laid out under uviol lamp, ultraviolet radiation 45min;
(2) it is 5h under 150KPa environment that the baikal skullcap root decoction pieces that (1) step has processed is placed in air pressure;
(3) by the baikal skullcap root decoction pieces after step (2) HIGH PRESSURE TREATMENT, the boiling water of 2 times of addition Radix Scutellariae weight, boil and carry 3 times, each 45min, filter, united extraction liquid, then extracting solution hydrochloric acid adjusts pH value to 1.5, precipitation baicalin precipitates, and rinses baicalin 3 times with circulating water, then under 50 DEG C of conditions, dry gained material is defined as crude baicalin in the present invention, according to the high-efficient liquid phase technique under 2010 editions Radix Scutellariae items of Chinese Pharmacopoeia, the amount of crude baicalin in radix scutellariae medicinal materials that measures is 143.2g, and extraction ratio is 71.6%.
HIGH PRESSURE TREATMENT concrete operations are: the baikal skullcap root decoction pieces after ultraviolet is processed loads in stainless steel cask, uses air compressor, squeezes into air, and the air pressure squeezing into stainless steel cask controls at 150KPa.

Claims (1)

1. a crude baicalin extraction process, it is characterised in that: comprise the following steps:
(1) take baikal skullcap root decoction pieces, evenly laid out under uviol lamp, ultraviolet radiation 30-45min;
(2) it is 3-5h under 120KPa to 150KPa environment that the baikal skullcap root decoction pieces that (1) step has processed is placed in air pressure;
(3) by the baikal skullcap root decoction pieces after step (2) HIGH PRESSURE TREATMENT, the boiling water of 1.5-2 times of addition Radix Scutellariae weight, boil and carry 2-3 time, each 45min, filters, united extraction liquid, then extracting solution hydrochloric acid adjusts pH value to 1.5, precipitates out baicalin precipitation, rinses baicalin 3 times with circulating water, then, under 40-50 DEG C of condition, dry gained material is defined as crude baicalin in the present invention.
CN201610125088.9A 2016-03-04 2016-03-04 Extraction technology for baicalin crude product Pending CN105669801A (en)

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CN201610125088.9A CN105669801A (en) 2016-03-04 2016-03-04 Extraction technology for baicalin crude product

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Application Number Priority Date Filing Date Title
CN201610125088.9A CN105669801A (en) 2016-03-04 2016-03-04 Extraction technology for baicalin crude product

Publications (1)

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CN105669801A true CN105669801A (en) 2016-06-15

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN107626220A (en) * 2016-07-19 2018-01-26 丁观军 A kind of method and its application for promoting flavones or glycosides compound dissolving

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN107626220A (en) * 2016-07-19 2018-01-26 丁观军 A kind of method and its application for promoting flavones or glycosides compound dissolving
CN107626220B (en) * 2016-07-19 2021-05-21 丁观军 Method for promoting dissolution of flavone or glycoside compounds and application thereof

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