CN100478348C - Method of separating and concentrating iridoid glycosides and crocin in cape jasmine fruit - Google Patents
Method of separating and concentrating iridoid glycosides and crocin in cape jasmine fruit Download PDFInfo
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- CN100478348C CN100478348C CNB2007100370973A CN200710037097A CN100478348C CN 100478348 C CN100478348 C CN 100478348C CN B2007100370973 A CNB2007100370973 A CN B2007100370973A CN 200710037097 A CN200710037097 A CN 200710037097A CN 100478348 C CN100478348 C CN 100478348C
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Abstract
The invention discloses a separating method of enriched iridoid glycosides component and saffron component, which comprises the following steps: extracting condensed cape jasmine extract through alcohol; adsorbing through large-hole resin; eluting and enriching through alcohol gradiently; decompressing; condensing to obtain the product.
Description
Technical field
The present invention relates to the enriching method of iridoids component and yellow pigment class component, particularly the method for separation and concentration iridoid glycosides component and crocin class component from cape jasmine fruit.
Background technology
The cape jasmine beginning is stated from Shennong's Herbal, classifies middle product as.Dry mature fruit for madder wort cape jasmine Gardeniajasminoides Ellis..Mainly be distributed in areas such as Jiangxi, Zhejiang, Hunan and Hubei.Gathered when 9～November, fruit maturation was reddish yellow.The property bitter cold, the thoughts of returning home, lung, tri-jiao channel.Has the purging intense heat relieving restlessness, clearing away heat and promoting diuresis, the effect of removing pattogenic heat from the blood and toxic material from the body.Cure mainly pyreticosis restlessness of asrhenia type and insomnia, jaundice, gonorrhoea, quench one's thirst, hot eyes, pharyngalgia, haematemesis, bleeding from five sense organs or subcutaneous tissue, bloody flux, hematuria, pathopyretic ulcer, sprain and swell and ache.
Discover, contain the number of chemical composition in the cape jasmine, wherein be mainly iridoid glycosides, organic acid and yellow pigment class etc.The iridoid glycoside compounds in the cape jasmine fruit wherein, its main component is jasminoidin (Geniposide), cape jasmine thuja acid (Geniposidic acid), gardoside (Gardoside), shanzhiside (Shanzhiside), Gardenoside (Gardenoside), cape jasmine ketoside (Gardosede) etc., has effects such as anti-inflammatory, analgesic, cholagogic and hypocatharsis.Contain the higher yellow pigment of content in the cape jasmine, its main component is crocin I (Crocin I), crocin II (Crocin II), crocin III (Crocin III) and crocetin (Crocetin) etc., crocin class pigment is unique water-soluble carotenoid that nature exists, and has effects such as anti-oxidant, cancellation free radical, anticancer growth.In addition, crocin class pigment good water solubility, strong to acid, alkali, salt equistability, nontoxicity, widespread use both at home and abroad is foodstuff additive and industrial dye, such as Noodles, carbohydrate, drinks is painted and as seasonings etc.
Iridoid glycoside and crocin etc. have better water solubility and pure dissolubility in the cape jasmine, therefore can adopt water extraction and alcohol extracting method to extract.The purification process that iridoid glycoside is commonly used has n-butanol extraction, neutral alumina chromatography, silica gel column chromatography etc., and these class methods are used more noxious solvent, has increased the aftertreatment of finished product and has detected step, and the cost of purge process is raise.Macroporous resin is well used at aspects such as middle pharmaceutically active ingredient or natural product extraction separation at present, macroporous resin also is applied in the purifying to Fructus Gardeniae extract, but method commonly used at present is not with iridoid glycoside and crocin comprehensive utilization, so there is the low shortcoming of medicinal material comprehensive utilization degree.
Summary of the invention
The objective of the invention is to overcome existing iridoid glycoside and crocin purification process toxicity is big, purification step is numerous and diverse, medicinal material is made a low multiple use shortcoming, a kind of environmental friendliness, easy and simple to handle, separation and concentration iridoid glycosides component from the cape jasmine medicinal material that the medicinal material comprehensive utilization ratio is high and the method for crocin class component are provided.
The present invention adopts macroporous adsorbent resin substep separation and concentration iridoid glycoside and crocin, and improvements are: 1, iridoid glycoside and crocin are focused on same separating unit, improve plant factor, reduce separation costs; 2, according to the polarity characteristics of iridoid glycoside and crocin with Different concentrations of alcohol to its wash-out, substep separation and concentration effective constituent improves the comprehensive utilization ratio of cape jasmine medicinal material.
The objective of the invention is to realize by the following technical solutions:
A kind of iridoid glycoside and crocin method for separating and concentrating may further comprise the steps:
(1) with the cape jasmine fruit meal with mass percent 50%～80% ethanol heating and refluxing extraction 15～60min in extraction equipment, solvent is doubly measured 8～12 times into crude drug meal quality, extracts 1～3 time.Obtain gardenia extract through centrifugal, filtration, be evaporated to 3～5 times of crude drug volume;
(2) will extract concentrated solution through absorption with macroporous adsorbent resin by the cape jasmine of step (1) gained, be 0～10% ethanol elution impurity with mass percent earlier, after use mass percent 25～35% and 50～70% ethanol through gradient elution respectively, promptly get iridoid glycosides component and crocin class component enriched substance behind the elutriant concentrate drying.
In above-mentioned steps (2), when using ethanol to carry out wash-out, the alcoholic acid usage quantity all is preferably 3～6 times of column volume.
Said macroporous resin optimization styrene macroporous adsorbent resin in the aforesaid method.
Iridoid glycosides component yield is 6.35%, and wherein jasminoidin content is 66.3%; Crocin class component yield is 4.42%, and wherein the content of crocin I is 14.0%.
The present invention adopt macroporous adsorbent resin at same separating unit to iridoid glycoside and crocin purifying, select the Different concentrations of alcohol gradient elution for use, the substep separation and concentration, improved plant factor, reduced separation costs, improved the overall utilization rate of medicinal material.Preparation technology of the present invention is simple, iridoid glycoside and crocin yield height, and cape jasmine medicinal material comprehensive utilization degree height is fit to suitability for industrialized production.
Description of drawings
Fig. 1 is an iridoid glycosides component high-efficient liquid phase chromatogram of the present invention (embodiment 1)
Fig. 2 is a crocin class component high-efficient liquid phase chromatogram of the present invention (embodiment 1)
Fig. 3 is the elution curve (embodiment 1) of jasminoidin in the iridoid glycosides component of the present invention
Fig. 4 is the elution curve (embodiment 1) of crocin I in the Stigma Croci class component of the present invention
Embodiment
Describe the present invention below in conjunction with embodiment and accompanying drawing.
Embodiment 1:
Get dry cape jasmine fruit meal 20g, measured 65% alcohol reflux 0.5 hour, filtration with 10 times.The dregs of a decoction were measured 65% alcohol reflux 0.5 hour with 10 times again, centrifugal, filtration, and merging filtrate, being evaporated to does not have the alcohol flavor, is settled to 4 times of crude drug volumes.
With the AB-8 resin 120ml that purifying the is good internal diameter 15mm that packs into, in the glass column of high 800mm.The 60ml gardenia extract that adds above-mentioned preparation gained.With the pure water of 5 times of bed volume, the flow velocity flush away water-soluble impurity of 1/2BV/h.Adopt 30%, 60% ethanol then respectively, carry out wash-out, collect elutriant with the 1/2BV/h flow velocity.Respectively with above-mentioned elutriant behind 50 ℃ of concentrating under reduced pressure, 60 ℃ of vacuum-dryings, obtaining iridoid glycosides component yield is 6.5%, wherein jasminoidin content is 65%; Crocin class component yield is 4.5%, and wherein the content of crocin I is 13%.
Embodiment 2:
Get dry cape jasmine fruit meal 600g, measure 65% alcohol reflux 3 times with 10 times, the extracting solution of gained is concentrated into about volume/crude drug ratio and is about 4: 1, centrifugal, supernatant liquor is immediately with sample on the 1/4BV/h flow velocity, after 5 times of bed volume washings,, and collect the iridoid glycoside part with 30% ethanol elution; Then with 60% ethanol elution and collect the crocin part.Jasminoidin solution and crocin solution are dried to constant weight in vacuum drying oven to thickness then in rotary evaporation below 60 ℃.Iridoid glycoside and crocin cut difference vacuum concentration drying with collecting get light yellow iridoid glycosides component powders 38.1g and sorrel crocin class component powders 26.5g.The yield of iridoid glycoside component is 6.35%, and wherein the jasminoidin content in the iridoid glycoside part is 66.3%; The yield of crocin component is 4.42%, and wherein crocin-I content is 14.0%.
Claims (3)
1, a kind of iridoid glycosides component and crocin class component method for separating and concentrating is characterized in that, said method comprising the steps of:
(1) with the cape jasmine fruit meal with mass percent 50%～80% ethanol heating and refluxing extraction 15～60 minutes in extraction equipment, solvent is doubly measured 8～12 times into crude drug meal quality, extract 1～3 time, obtain gardenia extract, be evaporated to 3～5 times of crude drug volume through centrifugal, filtration;
(2) will extract concentrated solution through absorption with macroporous adsorbent resin by the cape jasmine of step (1) gained, be 0～10% ethanol elution impurity with mass percent earlier, iridoid glycoside is separated with mass percent 25～35% ethanol elutions in the back, use mass percent 50～70% ethanol elutions again, separate crocin, promptly get iridoid glycoside and crocin class component enriched substance behind the elutriant concentrate drying.
2, a kind of method for separating and concentrating as claimed in claim 1 is characterized in that, in described step (2), used alcoholic acid usage quantity is 3～6 times of column volumes when carrying out wash-out.
3, a kind of method for separating and concentrating as claimed in claim 1 or 2 is characterized in that, said macroporous resin is the vinylbenzene macroporous adsorbent resin.
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| CNB2007100370973A CN100478348C (en) | 2007-02-02 | 2007-02-02 | Method of separating and concentrating iridoid glycosides and crocin in cape jasmine fruit |
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| CNB2007100370973A CN100478348C (en) | 2007-02-02 | 2007-02-02 | Method of separating and concentrating iridoid glycosides and crocin in cape jasmine fruit |
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| CN100478348C true CN100478348C (en) | 2009-04-15 |
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Families Citing this family (10)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN101863754A (en) * | 2009-04-17 | 2010-10-20 | 杭州法和医药科技有限公司 | Preparation method of crocetin, gardenia yellow pigment and saffron pigment |
| CN101940642B (en) * | 2010-10-08 | 2013-05-22 | 华东理工大学 | Chinese medicinal composition and application thereof |
| CN103039968A (en) * | 2012-10-31 | 2013-04-17 | 陈阳 | Formula of eyesight protecting heath care product and preparation method thereof |
| CN103387489B (en) * | 2013-07-11 | 2015-05-06 | 苏州大学 | Preparation method of high pure crocin and geniposide |
| CN103951718B (en) * | 2014-04-12 | 2016-03-30 | 云南云药医药研究有限公司 | A kind of method preparing high-purity gardenoside and crocin with cape jasmine |
| CN104398574A (en) * | 2014-10-22 | 2015-03-11 | 萧明尧 | Saffron crocus externally-applied ointment and preparation method thereof |
| CN105935363B (en) | 2016-04-29 | 2017-03-08 | 暨南大学 | Composition, safron class active site and application thereof |
| CN108752191A (en) * | 2018-08-28 | 2018-11-06 | 郑州中科新兴产业技术研究院 | The extracting method of crocin in a kind of efficient fast enriching Gardenia Yellow |
| CN109125258B (en) * | 2018-10-25 | 2020-09-18 | 华润三九（南昌）药业有限公司 | Preparation method of strong loquat syrup |
| CN113214674B (en) * | 2021-05-13 | 2022-11-15 | 湖南文理学院 | Multistage differentiation type-based device and method for extracting crocin from gardenia jasminoides ellis |
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2007
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| 吸附树脂AB - 8精制栀子黄色素的工艺研究. 谢凤霞等.南昌大学学报·工科版，第27卷第1期. 2005 |
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