CN104367622A - Method for extracting alkaloids from herba leonuri - Google Patents

Method for extracting alkaloids from herba leonuri Download PDF

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Publication number
CN104367622A
CN104367622A CN201410632570.2A CN201410632570A CN104367622A CN 104367622 A CN104367622 A CN 104367622A CN 201410632570 A CN201410632570 A CN 201410632570A CN 104367622 A CN104367622 A CN 104367622A
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China
Prior art keywords
herba leonuri
alkaloids
ethanol
filter
hydrochloric acid
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CN201410632570.2A
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陈兴权
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Changzhou University
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Changzhou University
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Priority to CN201410632570.2A priority Critical patent/CN104367622A/en
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    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K36/00Medicinal preparations of undetermined constitution containing material from algae, lichens, fungi or plants, or derivatives thereof, e.g. traditional herbal medicines
    • A61K36/18Magnoliophyta (angiosperms)
    • A61K36/185Magnoliopsida (dicotyledons)
    • A61K36/53Lamiaceae or Labiatae (Mint family), e.g. thyme, rosemary or lavender
    • A61K36/533Leonurus (motherwort)
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K2236/00Isolation or extraction methods of medicinal preparations of undetermined constitution containing material from algae, lichens, fungi or plants, or derivatives thereof, e.g. traditional herbal medicine
    • A61K2236/30Extraction of the material
    • A61K2236/33Extraction of the material involving extraction with hydrophilic solvents, e.g. lower alcohols, esters or ketones
    • A61K2236/333Extraction of the material involving extraction with hydrophilic solvents, e.g. lower alcohols, esters or ketones using mixed solvents, e.g. 70% EtOH
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K2236/00Isolation or extraction methods of medicinal preparations of undetermined constitution containing material from algae, lichens, fungi or plants, or derivatives thereof, e.g. traditional herbal medicine
    • A61K2236/50Methods involving additional extraction steps
    • A61K2236/53Liquid-solid separation, e.g. centrifugation, sedimentation or crystallization

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  • Health & Medical Sciences (AREA)
  • Natural Medicines & Medicinal Plants (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Alternative & Traditional Medicine (AREA)
  • Biotechnology (AREA)
  • Botany (AREA)
  • Medical Informatics (AREA)
  • Medicinal Chemistry (AREA)
  • Microbiology (AREA)
  • Mycology (AREA)
  • Pharmacology & Pharmacy (AREA)
  • Epidemiology (AREA)
  • Animal Behavior & Ethology (AREA)
  • General Health & Medical Sciences (AREA)
  • Public Health (AREA)
  • Veterinary Medicine (AREA)
  • Compounds Of Unknown Constitution (AREA)
  • Medicines Containing Plant Substances (AREA)

Abstract

The invention relates to a method for extracting alkaloids from herba leonuri. The method specifically comprises the steps of adding fresh herba leonuri into a constant-temperature furnace, drying in the presence of nitrogen, crushing and screening, carrying out ethanol soaking, ultrasonic washing and resin filtering, decompressing to recycle solvents, drying the solvents into paste by distillation, carrying out water-bath heating by virtue of hydrochloric acid and active carbon, carrying out elution, and finally carrying out compression concentration on an eluted solution, so as to obtain the alkaloids in herba leonuri.

Description

The extracting method of alkaloids in a kind of Herba Leonuri
Technical field
The present invention relates to a kind of extracting method, particularly the extracting method of alkaloids in a kind of Herba Leonuri.
Background technology
Herba Leonuri is one of conventional Chinese medicine, records in history tree detailed outline, belongs to Labiatae Herba Leonuri and belongs to various plants together, and the most frequently used be Herba Leonuri.Be used as medicine with the dry product of the aerial parts of bud stage or fresh goods, have the effect such as promoting blood flow to regulate menstruation, inducing diuresis to remove edema.Clinical menoxenia, vaginal bleeding during pregnancy difficult labour, dysmenorrhea and the postnatal blood stasis of being used for is suffered from abdominal pain, and have the title of " blood man panacea ", " multiparity good medicine ".Domestic and international numerous scholars have carried out long-term research to Herba Leonuri, obtain a lot of achievement, in Herba Leonuri, main chemical compositions contains alkaloids, flavonoid, organic acid, various trace elements and fatty acid etc., wherein studying more is alkaloids, and this is also have the bioactive element of the first species.Clinical conventional be Herba Leonuri raw medicinal herbs and motherwort formulation, its quality control take total alkaloids as index.
The extraction process of the alkaloids in Herba Leonuri all adopts the method for water extract-alcohol precipitation, concentrate drying always, and the effective component yield of the method is low, impure more, constrains and it is made modern dosage form further.
Summary of the invention
The present invention is directed to that traditional effective component yield is low, impurity content is high and affect the problems such as product quality, propose alkaloids extracting method in a kind of Herba Leonuri, the method effective component yield is high, without problems such as qualitative effects.
In order to reach above-mentioned purpose, the concrete technical scheme of employing is:
(1) fresh Herba Leonuri is put in constant temperature oven, under the protection of nitrogen at 50-55 DEG C dry 1-2h;
(2) dried Herba Leonuri is put in pulverizer pulverize, through sieving out 40-50 object motherwort powder;
(3) accurately take 3g motherwort powder and be placed in conical flask, add the ethanol that 20mL mass fraction is 95%, soak 1-2h, soak rear ultrasonic washing 2-3 time, then resin filter is used, filtrate decompression recycling design, then put it into transpiring moisture in Rotary Evaporators, until institute's extract matter is paste;
(4) add to it ethanol that 30mL mass fraction is 80%, supersound process 30min, lets cool, and in its weight of title, supply the weight of less loss, shake up with ethanol, filter, precision measures subsequent filtrate 25mL, heats to evaporating dish in water-bath;
(5) the hydrochloric acid solution 10mL that precision adds 0.15mol/L dissolves, and adds active carbon 0.5g, puts in water-bath and heat half a minute, agitation and filtration, in the 25mL volumetric flask of greenery, divide with the hydrochloric acid solution of 0.15mol/L and wash evaporating dish and filter 2 times, washing liquid is incorporated in same measuring bottle;
(6) carry out concentrating under reduced pressure at finally eluent being put in 70 DEG C, namely obtain the alkaloids in Herba Leonuri, alkaloids is placed in spectrophotometer and detects.
Specific embodiments
(1) fresh Herba Leonuri is put in constant temperature oven, under the protection of nitrogen at 50-55 DEG C dry 1-2h;
(2) dried Herba Leonuri is put in pulverizer pulverize, through sieving out 40-50 object motherwort powder;
(3) accurately take 3g motherwort powder and be placed in conical flask, add the ethanol that 20mL mass fraction is 95%, soak 1-2h, soak rear ultrasonic washing 2-3 time, then resin filter is used, filtrate decompression recycling design, then put it into transpiring moisture in Rotary Evaporators, until institute's extract matter is paste;
(4) add to it ethanol that 30mL mass fraction is 80%, supersound process 30min, lets cool, and in its weight of title, supply the weight of less loss, shake up with ethanol, filter, precision measures subsequent filtrate 25mL, heats to evaporating dish in water-bath;
(5) the hydrochloric acid solution 10mL that precision adds 0.15mol/L dissolves, and adds active carbon 0.5g, puts in water-bath and heat half a minute, agitation and filtration, in the 25mL volumetric flask of greenery, divide with the hydrochloric acid solution of 0.15mol/L and wash evaporating dish and filter 2 times, washing liquid is incorporated in same measuring bottle;
(6) carry out concentrating under reduced pressure at finally eluent being put in 70 DEG C, namely obtain the alkaloids in Herba Leonuri, alkaloids is placed in spectrophotometer and detects.
Example 1
Fresh Herba Leonuri is put in constant temperature oven, under the protection of nitrogen at 50 DEG C dry 1h; Dried Herba Leonuri is put in pulverizer and pulverizes, through sieving out 40 object motherwort powders; Accurately take 3g motherwort powder and be placed in conical flask, add the ethanol that 20mL mass fraction is 95%, soak 1h, soak rear ultrasonic washing 2 times, then used resin filter, filtrate decompression recycling design, put it into transpiring moisture in Rotary Evaporators again, until institute's extract matter is paste; Add to it ethanol that 30mL mass fraction is 80%, supersound process 30min, lets cool, and in its weight of title, supply the weight of less loss, shake up with ethanol, filter, precision measures subsequent filtrate 25mL, heats to evaporating dish in water-bath; The hydrochloric acid solution 10mL that precision adds 0.15mol/L dissolves, and adds active carbon 0.5g, puts in water-bath and heat half a minute, agitation and filtration, in the 25mL volumetric flask of greenery, divide with the hydrochloric acid solution of 0.15mol/L and wash evaporating dish and filter 2 times, washing liquid is incorporated in same measuring bottle; Carry out concentrating under reduced pressure at finally eluent being put in 70 DEG C, namely obtain the alkaloids in Herba Leonuri.
Example 2
Fresh Herba Leonuri is put in constant temperature oven, under the protection of nitrogen at 53 DEG C dry 1.5h; Dried Herba Leonuri is put in pulverizer and pulverizes, through sieving out 45 object motherwort powders; Accurately take 3g motherwort powder and be placed in conical flask, add the ethanol that 20mL mass fraction is 95%, soak 1.5h, soak rear ultrasonic washing 2 times, then used resin filter, filtrate decompression recycling design, put it into transpiring moisture in Rotary Evaporators again, until institute's extract matter is paste; Add to it ethanol that 30mL mass fraction is 80%, supersound process 30min, lets cool, and in its weight of title, supply the weight of less loss, shake up with ethanol, filter, precision measures subsequent filtrate 25mL, heats to evaporating dish in water-bath; The hydrochloric acid solution 10mL that precision adds 0.15mol/L dissolves, and adds active carbon 0.5g, puts in water-bath and heat half a minute, agitation and filtration, in the 25mL volumetric flask of greenery, divide with the hydrochloric acid solution of 0.15mol/L and wash evaporating dish and filter 2 times, washing liquid is incorporated in same measuring bottle; Carry out concentrating under reduced pressure at finally eluent being put in 70 DEG C, namely obtain the alkaloids in Herba Leonuri.
Example 3
Fresh Herba Leonuri is put in constant temperature oven, under the protection of nitrogen at 55 DEG C dry 2h; Dried Herba Leonuri is put in pulverizer and pulverizes, through sieving out 50 object motherwort powders; Accurately take 3g motherwort powder and be placed in conical flask, add the ethanol that 20mL mass fraction is 95%, soak 2h, soak rear ultrasonic washing 3 times, then used resin filter, filtrate decompression recycling design, put it into transpiring moisture in Rotary Evaporators again, until institute's extract matter is paste; Add to it ethanol that 30mL mass fraction is 80%, supersound process 30min, lets cool, and in its weight of title, supply the weight of less loss, shake up with ethanol, filter, precision measures subsequent filtrate 25mL, heats to evaporating dish in water-bath; The hydrochloric acid solution 10mL that precision adds 0.15mol/L dissolves, and adds active carbon 0.5g, puts in water-bath and heat half a minute, agitation and filtration, in the 25mL volumetric flask of greenery, divide with the hydrochloric acid solution of 0.15mol/L and wash evaporating dish and filter 2 times, washing liquid is incorporated in same measuring bottle; Carry out concentrating under reduced pressure at finally eluent being put in 70 DEG C, namely obtain the alkaloids in Herba Leonuri.

Claims (1)

1. the extracting method of alkaloids in Herba Leonuri, is characterized in that:
(1) fresh Herba Leonuri is put in constant temperature oven, under the protection of nitrogen at 50-55 DEG C dry 1-2h;
(2) dried Herba Leonuri is put in pulverizer pulverize, through sieving out 40-50 object motherwort powder;
(3) accurately take 3g motherwort powder and be placed in conical flask, add the ethanol that 20mL mass fraction is 95%, soak 1-2h, soak rear ultrasonic washing 2-3 time, then resin filter is used, filtrate decompression recycling design, then put it into transpiring moisture in Rotary Evaporators, until institute's extract matter is paste;
(4) add to it ethanol that 30mL mass fraction is 80%, supersound process 30min, lets cool, and in its weight of title, supply the weight of less loss, shake up with ethanol, filter, precision measures subsequent filtrate 25mL, heats to evaporating dish in water-bath;
(5) the hydrochloric acid solution 10mL that precision adds 0.15mol/L dissolves, and adds active carbon 0.5g, puts in water-bath and heat half a minute, agitation and filtration, in the 25mL volumetric flask of greenery, divide with the hydrochloric acid solution of 0.15mol/L and wash evaporating dish and filter 2 times, washing liquid is incorporated in same measuring bottle;
(6) carry out concentrating under reduced pressure at finally eluent being put in 70 DEG C, namely obtain the alkaloids in Herba Leonuri, alkaloids is placed in spectrophotometer and detects.
CN201410632570.2A 2014-11-11 2014-11-11 Method for extracting alkaloids from herba leonuri Pending CN104367622A (en)

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Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN105434278A (en) * 2015-12-30 2016-03-30 云南人羞花化妆品有限公司 Panax notoginseng toner and preparation method thereof
CN106729588A (en) * 2017-03-03 2017-05-31 四川德成动物保健品有限公司 Motherwort extraction process of effective component based on beneficial female biochemistry mixture
CN109180534A (en) * 2018-09-10 2019-01-11 合肥科佳高分子材料科技有限公司 A kind of method of Total alkaloids eluent desalination

Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1467204A (en) * 2002-07-10 2004-01-14 江苏康缘药业股份有限公司 Method for preparing motherwort total alkaloid and new medicine uses
CN101244121A (en) * 2007-02-15 2008-08-20 北京天新园医药科技开发有限公司 Leonurus heterophyllus total alkaloid extract and preparation thereof

Patent Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1467204A (en) * 2002-07-10 2004-01-14 江苏康缘药业股份有限公司 Method for preparing motherwort total alkaloid and new medicine uses
CN101244121A (en) * 2007-02-15 2008-08-20 北京天新园医药科技开发有限公司 Leonurus heterophyllus total alkaloid extract and preparation thereof

Non-Patent Citations (2)

* Cited by examiner, † Cited by third party
Title
付君叶: "利用超声法从益母草中提取总生物碱的研究", 《江西理工大学学报》 *
周本宏: "超声提取益母草总碱的工艺优选", 《医药导报》 *

Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN105434278A (en) * 2015-12-30 2016-03-30 云南人羞花化妆品有限公司 Panax notoginseng toner and preparation method thereof
CN106729588A (en) * 2017-03-03 2017-05-31 四川德成动物保健品有限公司 Motherwort extraction process of effective component based on beneficial female biochemistry mixture
CN109180534A (en) * 2018-09-10 2019-01-11 合肥科佳高分子材料科技有限公司 A kind of method of Total alkaloids eluent desalination
CN109180534B (en) * 2018-09-10 2021-04-23 合肥科佳高分子材料科技有限公司 Method for desalting motherwort total alkali eluent

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Application publication date: 20150225