CN101648956B - Method for extracting chlorophyll from silkworm excrement by using supercritical fluid - Google Patents
Method for extracting chlorophyll from silkworm excrement by using supercritical fluid Download PDFInfo
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- CN101648956B CN101648956B CN2009101701506A CN200910170150A CN101648956B CN 101648956 B CN101648956 B CN 101648956B CN 2009101701506 A CN2009101701506 A CN 2009101701506A CN 200910170150 A CN200910170150 A CN 200910170150A CN 101648956 B CN101648956 B CN 101648956B
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- silkworm excrement
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
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- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P20/00—Technologies relating to chemical industry
- Y02P20/50—Improvements relating to the production of bulk chemicals
- Y02P20/54—Improvements relating to the production of bulk chemicals using solvents, e.g. supercritical solvents or ionic liquids
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Abstract
The invention provides a method for extracting chlorophyll from silkworm excrement by using supercritical fluid, which comprises the following steps: sieving the silkworm excrement collected from a silkworm field or silkworm farmer, weighing 0.3-2g of silkworm excrement, adding water, softening the silkworm excrement for 1-6h, placing the silkworm excrement into an extraction kettle, leading in carbon dioxide, boosting the pressure to 18-30MPa through a high pressure pump, setting the temperature to be 30-65 DEG C and the flow of the carbon dioxide to be 40-150g/h, extracting for 1-4h, and obtaining the chlorophyll in a separator. Absolute ethyl alcohol can be added into an extractor to be used as an entrainer, the use amount of the entrainer is as follows: 0.05-0.15L of absolute ethyl alcohol is adopted in 1g of the raw material and the yield of the chlorophyll can reach 0.91 percent. The method greatly avoids reactions of de-magging, esterification and the like occurring in the process of common extraction, farthest keeps the original characteristics of the chlorophyll, has simple procedure, less steps, short production period, high efficiency, complete extraction and no any new three-wastes, and is beneficial to protecting the environment.
Description
Technical field
The invention belongs to separation field, relate in particular to a kind of method of utilizing supercutical fluid extracting chlorophyll from silkworm excrement.
Background technology
Pigment is a staining agent commonly used in food, medicine and the makeup.Along with improving constantly of standard of living, people throw doubt upon gradually to the chemosynthesis pigment, and the exploitation of natural pigment is more and more paid attention to.Chlorophyll is the natural food colour that China and most countries allow use.Chlorophyll distributes in plant materials in a large number, its derivative pharmaceutically have the wound healing of promotion, antiulcer agent, antitumor, antimicrobial, give protection against cancer, protect the liver, many-sided biological activity such as anti-anaemia.Chlorophyll is the green pigment in the photosynthetic membrane, and it is a capturing optical main component in the photosynthesis.Chlorophyll has four kinds of a, b, c and d.All plants that discharges oxygen when carrying out photosynthesis all contain chlorophyll a; Chlorophyll b is present in higher plant, green alga and the euglena; Chlorofucsin is present in diatom, haematococcus and the brown alga, and CHLOROPHYLL d is present in red algae.Chlorophyll in the higher plant chloroplast(id) mainly contains two kinds of chlorophyll a and chlorophyll bs.The molecular structure of chlorophyll a by 4 pyrrole rings by 4 methenes (=CH-) be connected to form ring texture, be called porphyrin (side chain is arranged on the ring).Porphyrin ring is central in conjunction with 1 magnesium atom, and a cyclopentanone (V) is arranged, and the propionic acid on ring IV is by phytol (C
20H
39OH) it is water-soluble to form the sylvite tool after esterification, the saponification.They are water insoluble, and are dissolved in organic solvent, as ethanol, acetone, ether, chloroform etc.
Chlorophyll can activating cells metabolism, anti-oxidant, suppress the damage of oxyradical cell membrane; To various enzymes particularly trypsinase restraining effect is arranged; Blood sugar regulation; Promote hematopoietic function; Detoxifcation, antianaphylaxis, anticomplement; Vasodilation, microcirculation improvement; Deodorize, promote granulation new life and wound healing; Antitumous effect can effectively suppress the carcinogenesis of aflatoxin.
Silkworm excrement is the ight soil of silkworm, wherein contains a large amount of chlorophyll, protein closes pectin, is to extract chlorophyllous cheap, the raw material that is easy to get.Tradition is extracted chlorophyllous operation and is comprised from silkworm excrement: lixiviate, saponification, acid out, washing, complexing etc.Lixiviate organic solvent commonly used has ethanol, acetone, sherwood oil, chloroform, benzene etc.But traditional chlorophyll extracting method complex process, long flow path, most organic solvents are unfavorable and environment is unfriendly to health, and not only the extracting and separating solvent is very bothersome, and dissolvent residual is inevitable; Extraction temperature height, time is long, chlorophyll is damaged easily, in leaching process, usually take place especially with reactions such as de-magging, esterifications, consequently not only make quality product be difficult to stable control, and changed chlorophyllous natural characteristic, brought a series of uncertain factor for later application; Because tradition is extracted static extractions of adopting more, exists the problem of equilibrium concentration restriction, thereby is difficult to accomplish to extract fully, it is low to extract productive rate, poor selectivity, and waste is serious; Whole leaching process relates to the multistep phase transformation, need a large amount of heat of phase transformation, thereby energy consumption is bigger.
And the essential characteristic of supercritical liquid extraction technique is with fluid nontoxic, noresidue, as CO
2, replace organic solvent is done to extract medium and extract under the condition near room temperature; Its physical chemistry basis comes from supercritical CO
2The fluidic solvent property can be regulated and control in very wide scope, just can make solute at supercritical CO as long as change the temperature or the pressure of system simply
2Very big change takes place in solubleness in the fluid, thus for the highly selective extraction with separate and high-quality product provides possible; Its biggest advantage has been simplified technical process greatly no more than a plurality of unit processes such as extraction, separation and removal solvent being integrated, and has improved production efficiency, and environment is not polluted.Benefit is as follows: CO
2Colourless, tasteless, nontoxic, and be gas under the usual conditions, the no solvent residue problem makes healthy the obtaining of pure natural raw material that be perfectly safe become easy thing and CO with it as extraction agent
2Cheap and easy to get, can be recycled, the cost of product is greatly reduced; Extraction temperature is near room temperature, and whole extraction separation process is carried out in details in a play not acted out on stage, but told through dialogues, and chlorophyll has been avoided reactions such as recurrent de-magging, esterification in the conventional leaching process to a great extent to photaesthesia, can farthest keep the original characteristic of chlorophyll; Flow process is simple, and step is few, and is with short production cycle, the efficient height; Supercritical CO
2Fluidic dissolving power and seepage force are strong, and rate of diffusion is fast, and the chlorophyll product constantly is removed, and extract fully; Supercritical CO
2Fluid only works to solute, does not change any composition or raw material matrix outside the solute, therefore can not produce any new " three wastes " material, and is very favourable to environment protection.
I am once at " supercritical CO
2Chlorophyll in the extraction mao bamboon leaf " (Beijing University of Chemical Technology's journal, 2007,34 (1): be raw material with the mao bamboon leaf 92-94), studied and used supercritical CO
2Abstraction technique is extracting chlorophyll from the mao bamboon leaf, but chlorophyllous yield only is 0.32% under optimum process condition, and the leaf of bamboo needs natural air drying, pulverizing, and this can make chlorophyll lose in treating processes, and chlorophyllous yield is not high.
Summary of the invention
Technical problem to be solved by this invention is to overcome above-mentioned defective, and a kind of method of utilizing supercutical fluid extracting chlorophyll from silkworm excrement is provided.It comprises the steps: the silkworm excrement well sifted of collecting by silkworm field or silkworm raiser, add water softening 1-6 hour behind the weighing 0.3-2g, silkworm excrement is put into extraction kettle, feed carbonic acid gas, boost to 18-30Mpa by high-pressure pump, temperature is set at 30-65 ℃, and the flow of carbonic acid gas is 40-150g/h, extracted 1-4 hour, with separator that extraction kettle links to each other in obtain chlorophyll.
Preferably, add dehydrated alcohol as entrainment agent in extractor, the consumption of entrainment agent is the dehydrated alcohol that every gram raw material adopts 0.05-0.15L.
Can adopt spectrophotometry chlorophyll, that is: after extraction experiments finishes, in separator, add small amount of ethanol, the rolling flow separator is dissolved in ethanol with the chlorophyll product, ethanolic soln is poured in the 25ml volumetric flask then, in separator, add the small amount of ethanol flushing once more, washing fluid is poured in the last volumetric flask equally, youngster is inferior so repeatedly, product all dissolves and pours in the volumetric flask in separator, be settled to 25ml in volumetric flask, adding ethanol, dissolving evenly the back place 10 minutes standby.Solution to be measured is added in the cuvette, and as blank solution, in the interscan of 550nm-700nm wavelength, the scanning back is arrived as the product solution abosrption spectrogram with ethanol.Absorbancy under record 664nm and the 645nm wavelength.
Utilize experimental formula to calculate chlorophyll-a concentration, chlorophyll b concentration, chlorophyll total concn and chlorophyll yield:
Chlorophyll-a concentration: C
a=12.7A
664-2.69A
645
Chlorophyll b concentration: C
b=22.9A
645-4.68A
664
Chlorophyll total concn: C
A+b=C
a+ C
b
Chlorophyll yield=(extract total chlorophyll amount/g)/(material quantity/g)
A in the formula
664, A
645Represent the absorbancy of specimen under 664nm and 645nm wavelength respectively; C
a, C
bRepresent chlorophyll a and chlorophyll b concentration, unit is mg/L.
Description of drawings
Fig. 1 is a process flow diagram of the present invention.
A-CO wherein
2Steel cylinder; The B-Controlling System; C-is used for the high-pressure pump of transport of carbon dioxide; The D-temperature controlling system; E-is used for carrying the high-pressure pump of entrainment agent; The F-extraction kettle; The G-separator.
Specific embodiment
Embodiment 1:
Get 1g behind the silkworm excrement well sifted that will collect by silkworm field or silkworm raiser, added water softening 4 hours, silkworm excrement is put into extraction kettle F, by steel cylinder A carbonic acid gas is input among the extraction kettle F, utilize Controlling System B control extraction conditions, wherein boost to 25Mpa by high-pressure pump C, by temperature controlling system D temperature is set at 50 ℃, the flow of carbonic acid gas is 60g/h, extracted 4 hours, add dehydrated alcohol as entrainment agent with high-pressure pump E in extractor, the consumption of entrainment agent is the dehydrated alcohol that every gram raw material adopts 0.1L, obtains chlorophyll in separator G.Adopt spectrophotometry chlorophyll, drawing the chlorophyll yield is 0.73%, and wherein the concentration of chlorophyll a accounts for 12% of total chlorophyll concentration, and chlorophyll b concentration accounts for 88% of total chlorophyll concentration.
Embodiment 2:
Get 0.5g behind the silkworm excrement well sifted that will collect by silkworm field or silkworm raiser, added water softening 1 hour, silkworm excrement is put into extraction kettle F, by steel cylinder A carbonic acid gas is input among the extraction kettle F, utilize Controlling System B control extraction conditions, wherein boost to 18Mpa by high-pressure pump C, by temperature controlling system D temperature is set at 40 ℃, the flow of carbonic acid gas is 40g/h, extracted 3 hours, add dehydrated alcohol as entrainment agent with high-pressure pump E in extractor, the consumption of entrainment agent is the dehydrated alcohol that every gram raw material adopts 0.05L, obtains chlorophyll in separator G.Adopt spectrophotometry chlorophyll, drawing the chlorophyll yield is 0.57%, and wherein the concentration of chlorophyll a accounts for 8% of total chlorophyll concentration, and chlorophyll b concentration accounts for 92% of total chlorophyll concentration.
Embodiment 3:
Get 1g behind the silkworm excrement well sifted that will collect by silkworm field or silkworm raiser, added water softening 3 hours, silkworm excrement is put into extraction kettle F, by steel cylinder A carbonic acid gas is input among the extraction kettle F, utilize Controlling System B control extraction conditions, wherein boost to 30Mpa by high-pressure pump C, by temperature controlling system D temperature is set at 60 ℃, the flow of carbonic acid gas is 120g/h, extracted 2 hours, add dehydrated alcohol as entrainment agent with high-pressure pump E in extractor, the consumption of entrainment agent is the dehydrated alcohol that every gram raw material adopts 0.15L, obtains chlorophyll in separator.Adopt spectrophotometry chlorophyll, drawing the chlorophyll yield is 0.81%, and wherein the concentration of chlorophyll a accounts for 13% of total chlorophyll concentration, and chlorophyll b concentration accounts for 87% of total chlorophyll concentration.
Claims (2)
1. method of utilizing supercutical fluid extracting chlorophyll from silkworm excrement, it is characterized in that comprising the steps: the silkworm excrement well sifted of collecting with by silkworm field or silkworm raiser, add water softening 1-6 hour behind the weighing 0.3-2g, silkworm excrement is put into extraction kettle, feed carbonic acid gas, boost to 18-30Mpa by high-pressure pump, temperature is set at 30-65 ℃, the flow of carbonic acid gas is 40-150g/h, extracted 1-4 hour, with separator that extraction kettle links to each other in obtain chlorophyll.
2. method according to claim 1 is characterized in that adding dehydrated alcohol as entrainment agent in extraction kettle, the consumption of entrainment agent is the dehydrated alcohol that every gram silkworm excrement adopts 0.05-0.15L.
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| CN2009101701506A CN101648956B (en) | 2009-09-04 | 2009-09-04 | Method for extracting chlorophyll from silkworm excrement by using supercritical fluid |
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| CN2009101701506A CN101648956B (en) | 2009-09-04 | 2009-09-04 | Method for extracting chlorophyll from silkworm excrement by using supercritical fluid |
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| CN101648956A CN101648956A (en) | 2010-02-17 |
| CN101648956B true CN101648956B (en) | 2011-12-14 |
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| CN103965205B (en) * | 2014-05-29 | 2016-08-24 | 山东广通宝医药有限公司 | A kind of supercritical purifies the method producing chlorophyll copper sodium |
| CN105777762A (en) * | 2014-12-24 | 2016-07-20 | 北京化工大学常州先进材料研究院 | Method for extracting chlorophyll from phyllostachys pubescens leaves by utilization of supercritical fluid |
| CN105777761A (en) * | 2014-12-24 | 2016-07-20 | 北京化工大学常州先进材料研究院 | Supercritical fluid method for extraction of chlorophyll from green bamboo leaves |
| CN105777763A (en) * | 2014-12-25 | 2016-07-20 | 北京化工大学常州先进材料研究院 | Method for extracting chlorophyll from indocalamus leaves by means of supercritical fluid |
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Owner name: JIANGSU C-JUN BIOTECHNOLOGY CO., LTD. Free format text: FORMER OWNER: CHANGZHOU INSTITUTE OF ADVANCED MATERIAL, BEIJING UNIVERSITY OF CHEMICAL TECHNOLOGY Effective date: 20150818 |
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Effective date of registration: 20150818 Address after: 213164 Changzhou City, Wujin province Chang Wu Road, No. 18, No. Patentee after: Jiangsu Jun Bang cutting-edge biotechnology Co., Ltd. Address before: 213164 No. 801 middle Wu Road, Changzhou, Jiangsu Patentee before: Changzhou Institute of Advanced Material, Beijing University of Chemical Technology |
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Granted publication date: 20111214 Termination date: 20160904 |