CN115028668B - Extraction process of crocin - Google Patents
Extraction process of crocin Download PDFInfo
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- CN115028668B CN115028668B CN202210675813.5A CN202210675813A CN115028668B CN 115028668 B CN115028668 B CN 115028668B CN 202210675813 A CN202210675813 A CN 202210675813A CN 115028668 B CN115028668 B CN 115028668B
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- C07—ORGANIC CHEMISTRY
- C07H—SUGARS; DERIVATIVES THEREOF; NUCLEOSIDES; NUCLEOTIDES; NUCLEIC ACIDS
- C07H1/00—Processes for the preparation of sugar derivatives
- C07H1/06—Separation; Purification
- C07H1/08—Separation; Purification from natural products
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- C07H13/04—Compounds containing saccharide radicals esterified by carbonic acid or derivatives thereof, or by organic acids, e.g. phosphonic acids by carboxylic acids having the esterifying carboxyl radicals attached to acyclic carbon atoms
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Abstract
The invention discloses an extraction process of crocin, which mainly comprises the following steps: grinding stigma croci Sativi, adding extraction solvent, extracting in a microwave extraction tank, collecting extractive solution, purifying and adsorbing with chromatography column filled with molecular engram polymer microsphere of stigma croci Sativi glycoside, collecting eluate, concentrating, and drying to obtain stigma croci Sativi glycoside. The molecular engram polymer microsphere used in the invention has good selective adsorptivity and strong specificity to crocin, and the extraction liquid is adsorbed by using the chromatographic column filled with the molecular engram polymer microsphere, so that the aim of impurity removal and purification can be achieved, and the extraction rate of the product is high, and the purity is good.
Description
Technical Field
The invention relates to the technical field of natural product extraction. More particularly, the invention relates to an extraction process of crocin.
Background
Saffron is also called crocus sativus and crocus sativus, is a rare Chinese medicinal material, has strong physiological activity, has the effects of tranquilizing, eliminating phlegm and relieving spasm in Asia and Europe, and is used for treating gastropathy, menstruation regulating, measles, fever, yellow gall, hepatosplenomegaly, etc. The crocin in the saffron has better water solubility and alcohol solubility, and is generally extracted by water, alcohol or solutions with different alcohol concentrations, wherein the extraction method comprises a reflux method, a standing method, an ultrasonic method and the like, and then the saffron is purified by a silica gel chromatographic column method, a crystallization method, a two-phase solvent extraction method and a macroporous resin method, and the preparation process generally requires higher temperature or longer time, and has higher production cost, low extraction rate and low product purity.
Disclosure of Invention
It is an object of the present invention to solve at least the above problems and to provide at least the advantages to be described later.
The invention also aims to provide an extraction process of crocin, which has the advantages of good selectivity, high extraction rate, good stability, simple process flow and convenient operation.
To achieve these objects and other advantages and in accordance with the purpose of the invention, there is provided a process for extracting crocin, comprising the steps of: grinding stigma croci Sativi, adding extraction solvent, extracting in a microwave extraction tank, collecting extractive solution, purifying and adsorbing with chromatography column filled with molecular engram polymer microsphere of stigma croci Sativi glycoside, collecting eluate, concentrating, and drying to obtain stigma croci Sativi glycoside.
Preferably, the preparation method of the saffron crocin molecularly imprinted polymer microsphere mainly comprises the following steps:
step one, feCl 3 ·6H 2 O is dissolved in citric acid solution, ethylene glycol is added as dispersing agent, heating is carried out for 1-5h at 65-80 ℃ to form ferric oxide sol, the ferric oxide sol is mixed with silicon dioxide sol to obtain mixed sol, urea and formaldehyde are added, heating, filtering and drying are carried out, calcining is carried out for 5-8h at 500-1000 ℃ to obtain magnetic silica gel microsphere, wherein the mole ratio of silicon dioxide sol, ferric oxide sol, urea and formaldehyde is (20-40): 1 (5-10): 8-15);
step two, the molar ratio is (1-2): 1 and itaconic acid are mixed, heated for 30-90 min at 50-100 ℃ to prepare choline chloride-itaconic acid, and crocin and choline chloride-itaconic acid are mixed according to a mole ratio of 1: (5-10) dissolving in ethanol solution, adding azodiisobutyronitrile and ethylene glycol dimethacrylate, and 1-butyl-3-methylimidazole tetrafluoroborate, and introducing nitrogen to prepare a mixed solution, wherein the mol ratio of the azodiisobutyronitrile to the ethylene glycol dimethacrylate, the 1-butyl-3-methylimidazole tetrafluoroborate to the choline chloride-itaconic acid is (1-3): (4-6): (10-15): 1;
immersing the magnetic silica gel microsphere prepared in the first step into the mixed solution prepared in the second step, performing ultrasonic dispersion at 60 ℃ until polymerization is complete, taking out the microsphere, and washing the microsphere with methanol and acetic acid solution with the volume ratio of 9:1 to prepare the saffron glucoside molecularly imprinted polymer microsphere.
Preferably, the calcination temperature in the first step is 800 ℃ and the calcination time is 6 hours.
Preferably, the specific steps of purifying and adsorbing the extracting solution are as follows:
step a, loading the saffron glucoside molecularly imprinted polymer microspheres into a chromatographic column, and prepressing for 8-10h by using petroleum ether as a mobile phase;
b, injecting the extract liquid obtained after saffron extraction into a chromatographic column for purification and adsorption, wherein the eluent is petroleum ether, the flow rate is 0.5-1 ml/min, collecting the eluent, and measuring the absorbance;
and c, replacing ethanol as eluent to wash the chromatographic column, collecting eluent, concentrating and drying to finally obtain the crocin.
Preferably, the extraction solvent is one or more of water, ethanol and propylene glycol.
Preferably, the average particle size of the saffron crocin molecularly imprinted polymer microsphere is 30-100 μm.
The invention at least comprises the following beneficial effects: according to the extraction process of the crocin, disclosed by the invention, the crocin is extracted by utilizing the microwave extraction process, and then the crocin is selectively adsorbed by combining the chromatographic column filled with the crocin molecular engram polymer microspheres, so that the finally collected crocin product is high in extraction rate and good in purity, and the crocin molecular engram polymer microspheres can be reused, so that the cost is saved, and the resources are saved.
Additional advantages, objects, and features of the invention will be set forth in part in the description which follows and in part will become apparent to those having ordinary skill in the art upon examination of the following or may be learned from practice of the invention.
Detailed Description
The present invention is described in further detail below to enable those skilled in the art to practice the invention by reference to the specification.
It will be understood that terms, such as "having," "including," and "comprising," as used herein, do not preclude the presence or addition of one or more other elements or groups thereof.
The experimental methods described in the following embodiments are conventional methods unless otherwise indicated, and the reagents and materials are commercially available.
Example 1 ]
Grinding and crushing saffron, adding the saffron into a mixed solution of ethanol and water, placing the mixed solution into a microwave extraction tank for extraction, and collecting an extracted extract;
step two, taking microspheres prepared by using a crocin molecularly imprinted polymer as a stationary phase, mixing choline chloride and itaconic acid with a molar ratio of 1.5:1, heating for 60min at 80 ℃ to prepare choline chloride-itaconic acid, dissolving crocin and choline chloride-itaconic acid in an ethanol solution according to a molar ratio of 1:8, adding azodiisobutyronitrile and ethylene glycol dimethacrylate and 1-butyl-3-methylimidazole tetrafluoroborate, introducing nitrogen to prepare a mixed solution, wherein the molar ratio of azodiisobutyronitrile to ethylene glycol dimethacrylate and 1-butyl-3-methylimidazole tetrafluoroborate to choline chloride-itaconic acid is 1.5:5:12:1, heating to 60 ℃ to perform ultrasonic dispersion until complete polymerization, taking out the microspheres, and washing with methanol and acetic acid solution with a volume ratio of 9:1 to prepare the crocin molecularly imprinted polymer microspheres;
filling the saffron crocin molecularly imprinted polymer microspheres into a chromatographic column, and prepressing for 10 hours by using petroleum ether as a mobile phase;
step four, sampling the extract liquid obtained after saffron extraction into a chromatographic column, purifying and adsorbing, wherein the eluent is petroleum ether, the flow rate is 0.5ml/min, collecting the eluent, and measuring the absorbance;
and fifthly, replacing ethanol as eluent to wash the chromatographic column, collecting eluent, concentrating and drying to finally obtain the crocin.
Example 2 ]
Grinding and crushing saffron, adding the saffron into a mixed solution of ethanol and propylene glycol, placing the mixed solution into a microwave extraction tank for extraction, and collecting an extracted extract;
step two, feCl is added 3 ·6H 2 O is dissolved in citric acid solution, ethylene glycol is added as a dispersing agent, heating is carried out for 2 hours at 80 ℃ to form ferric oxide sol, the ferric oxide sol is mixed with silicon dioxide sol to obtain mixed sol, urea and formaldehyde are added, heating, filtering, drying and calcining are carried out for 6 hours at 800 ℃ to obtain magnetic silica gel microspheres, wherein the molar ratio of the silicon dioxide sol to the ferric oxide sol to the urea to the formaldehyde is 25:1:6:10;
step three, mixing choline chloride and itaconic acid with a molar ratio of 1.5:1, heating for 60min at 80 ℃ to prepare choline chloride-itaconic acid, dissolving crocin and choline chloride-itaconic acid into ethanol solution with a molar ratio of 1:8, adding azodiisobutyronitrile and ethylene glycol dimethacrylate and 1-butyl-3-methylimidazole tetrafluoroborate, and introducing nitrogen to prepare a mixed solution, wherein the molar ratio of azodiisobutyronitrile to ethylene glycol dimethacrylate and 1-butyl-3-methylimidazole tetrafluoroborate to choline chloride-itaconic acid is 2:5.5:12:1;
immersing the magnetic silica gel microsphere prepared in the first step into the mixed solution prepared in the second step, performing ultrasonic dispersion at 60 ℃ until polymerization is complete, taking out the microsphere, and washing the microsphere with methanol and acetic acid solution with the volume ratio of 9:1 to prepare the saffron glucoside molecularly imprinted polymer microsphere.
Fifthly, filling the saffron glucoside molecularly imprinted polymer microsphere into a chromatographic column, and prepressing for 10 hours by using petroleum ether as a mobile phase;
step six, injecting the extract liquid obtained after saffron extraction into a chromatographic column for purification and adsorption, wherein the eluent is petroleum ether, the flow rate is 0.8ml/min, collecting the eluent, and measuring the absorbance;
and seventhly, replacing ethanol as eluent to wash the chromatographic column, collecting eluent, concentrating and drying to finally obtain the crocin.
Example 3 ]
Grinding and crushing saffron, adding the saffron into a mixed solution of ethanol and propylene glycol, placing the mixed solution into a microwave extraction tank for extraction, and collecting an extracted extract;
step two, feCl is added 3 ·6H 2 O is dissolved in citric acid solution, ethylene glycol is added as a dispersing agent, heating is carried out for 1h at 65 ℃ to form ferric oxide sol, the ferric oxide sol is mixed with silicon dioxide sol to obtain mixed sol, urea and formaldehyde are added, heating, filtering, drying and calcining are carried out for 5h at 500 ℃ to obtain magnetic silica gel microspheres, wherein the molar ratio of the silicon dioxide sol to the ferric oxide sol to the urea to the formaldehyde is 20:1:5:8;
step three, mixing choline chloride and itaconic acid with a molar ratio of 1:1, heating for 30min at 50 ℃ to prepare choline chloride-itaconic acid, dissolving crocin and choline chloride-itaconic acid into ethanol solution with a molar ratio of 1:5, adding azodiisobutyronitrile and ethylene glycol dimethacrylate and 1-butyl-3-methylimidazole tetrafluoroborate, and introducing nitrogen to prepare a mixed solution, wherein the molar ratio of azodiisobutyronitrile to ethylene glycol dimethacrylate and 1-butyl-3-methylimidazole tetrafluoroborate to choline chloride-itaconic acid is 1:4:10:1;
immersing the magnetic silica gel microsphere prepared in the first step into the mixed solution prepared in the second step, performing ultrasonic dispersion at 60 ℃ until polymerization is complete, taking out the microsphere, and washing the microsphere with methanol and acetic acid solution with the volume ratio of 9:1 to prepare the saffron glucoside molecularly imprinted polymer microsphere.
Fifthly, filling the saffron glucoside molecularly imprinted polymer microsphere into a chromatographic column, and prepressing for 10 hours by using petroleum ether as a mobile phase;
step six, injecting the extract liquid obtained after saffron extraction into a chromatographic column for purification and adsorption, wherein the eluent is petroleum ether, the flow rate is 0.8ml/min, collecting the eluent, and measuring the absorbance;
and seventhly, replacing ethanol as eluent to wash the chromatographic column, collecting eluent, concentrating and drying to finally obtain the crocin.
Example 4 ]
Grinding and crushing saffron, adding the saffron into a mixed solution of ethanol and propylene glycol, placing the mixed solution into a microwave extraction tank for extraction, and collecting an extracted extract;
step two, feCl is added 3 ·6H 2 O is dissolved in citric acid solution, ethylene glycol is added as a dispersing agent, heating is carried out for 5 hours at 80 ℃ to form ferric oxide sol, the ferric oxide sol is mixed with silicon dioxide sol to obtain mixed sol, urea and formaldehyde are added, heating, filtering, drying and calcining are carried out for 8 hours at 1000 ℃ to obtain magnetic silica gel microspheres, wherein the mole ratio of the silicon dioxide sol to the ferric oxide sol to the urea to the formaldehyde is 40:1:10:15;
step three, mixing choline chloride and itaconic acid with a molar ratio of 2:1, heating for 90min at 100 ℃ to prepare choline chloride-itaconic acid, dissolving crocin and choline chloride-itaconic acid into an ethanol solution according to a molar ratio of 1:10, adding azodiisobutyronitrile and ethylene glycol dimethacrylate and 1-butyl-3-methylimidazole tetrafluoroborate, and introducing nitrogen to prepare a mixed solution, wherein the molar ratio of azodiisobutyronitrile to ethylene glycol dimethacrylate and 1-butyl-3-methylimidazole tetrafluoroborate to choline chloride-itaconic acid is 3:6:15:1;
immersing the magnetic silica gel microsphere prepared in the first step into the mixed solution prepared in the second step, performing ultrasonic dispersion at 60 ℃ until polymerization is complete, taking out the microsphere, and washing the microsphere with methanol and acetic acid solution with the volume ratio of 9:1 to prepare the saffron glucoside molecularly imprinted polymer microsphere.
Fifthly, filling the saffron glucoside molecularly imprinted polymer microsphere into a chromatographic column, and prepressing for 10 hours by using petroleum ether as a mobile phase;
step six, injecting the extract liquid obtained after saffron extraction into a chromatographic column for purification and adsorption, wherein the eluent is petroleum ether, the flow rate is 0.8ml/min, collecting the eluent, and measuring the absorbance;
and seventhly, replacing ethanol as eluent to wash the chromatographic column, collecting eluent, concentrating and drying to finally obtain the crocin.
Comparative example 1 ]
A process for extracting crocin includes such steps as grinding saffron, adding it to the mixture of alcohol and propanediol, extracting in microwave extracting tank, collecting the extracted liquid, filtering, washing, concentrating by rotary evaporation, and drying.
Comparative example 2 ]
The extraction process of crocin is the same as in example 2, except that the purification and adsorption are carried out only by using a chromatographic column filled with crocin molecularly imprinted polymer microspheres, and the specific steps are as follows:
grinding saffron, adding water, filtering, and collecting filtrate;
step two, feCl is added 3 ·6H 2 O is dissolved in citric acid solution, glycol is added as dispersing agent,heating at 80 ℃ for 2 hours to form ferric oxide sol, mixing the ferric oxide sol with silicon dioxide sol to obtain mixed sol, adding urea and formaldehyde, heating, filtering, drying, calcining at 800 ℃ for 6 hours to obtain magnetic silica gel microspheres, wherein the molar ratio of the silicon dioxide sol to the ferric oxide sol to the urea to the formaldehyde is 25:1:6:10;
step three, mixing choline chloride and itaconic acid with a molar ratio of 1.5:1, heating for 60min at 80 ℃ to prepare choline chloride-itaconic acid, dissolving crocin and choline chloride-itaconic acid into ethanol solution with a molar ratio of 1:8, adding azodiisobutyronitrile and ethylene glycol dimethacrylate and 1-butyl-3-methylimidazole tetrafluoroborate, and introducing nitrogen to prepare a mixed solution, wherein the molar ratio of azodiisobutyronitrile to ethylene glycol dimethacrylate and 1-butyl-3-methylimidazole tetrafluoroborate to choline chloride-itaconic acid is 2:5.5:12:1;
immersing the magnetic silica gel microsphere prepared in the first step into the mixed solution prepared in the second step, performing ultrasonic dispersion at 60 ℃ until polymerization is complete, taking out the microsphere, and washing the microsphere with methanol and acetic acid solution with the volume ratio of 9:1 to prepare the saffron glucoside molecularly imprinted polymer microsphere.
Fifthly, filling the saffron glucoside molecularly imprinted polymer microsphere into a chromatographic column, and prepressing for 10 hours by using petroleum ether as a mobile phase;
step six, injecting the filtrate collected in the step one into a chromatographic column for purification and adsorption, wherein the eluent is petroleum ether, the flow rate is 0.8ml/min, collecting the eluent, and measuring the absorbance;
and seventhly, replacing ethanol as eluent to wash the chromatographic column, collecting eluent, concentrating and drying to finally obtain the crocin.
Comparative example 3 ]
The crocin is extracted by a traditional method, and the specific process is as follows: grinding stigma croci Sativi, adding water, filtering, collecting filtrate, loading onto HPD-100a macroporous resin chromatographic column, eluting with petroleum ether to remove impurities, eluting with ethanol, collecting ethanol eluate, concentrating, and drying to obtain crocin.
< crocin extraction yield test >
The extraction rates of crocin obtained in each of examples and comparative examples were measured, and the results are shown in Table 1. As can be seen from Table 1, the extraction rates of examples 1 to 4 are significantly higher than those of comparative examples 1 to 3, which demonstrates that the extraction process of crocin according to the present invention can be used to obtain crocin with high extraction rate and high yield. In addition, the reason that the extraction rate of examples 2 to 4 is further higher than that of example 1 is that the microspheres prepared from the crocin molecularly imprinted polymer per se are used as the stationary phase in example 1, and are limited by the technical process and equipment, the uniformity of the particle size of the microspheres is poor, so that the uniformity is poor when a chromatographic column is filled, while the method of grafting polymerization on the surface of the silica gel microspheres is adopted in examples 2 to 4, and the particle size of the prepared crocin molecularly imprinted polymer microspheres is also uniform on the basis of the uniformity of the particle size of the silica gel microspheres, so that the extraction rate of crocin is further improved.
TABLE 1
| Extraction rate | |
| Example 1 | 28％ |
| Example 2 | 30％ |
| Example 3 | 29％ |
| Example 4 | 32％ |
| Comparative example 1 | 15％ |
| Comparative example 2 | 22％ |
| Comparative example 3 | 20％ |
< saffron glycoside purity test >
TABLE 2
| Purity of | |
| Example 1 | 92.7％ |
| Example 2 | 95.3％ |
| Example 3 | 94.9％ |
| Example 4 | 95.4％ |
| Comparative example 1 | 38.8％ |
| Comparative example 2 | 52.6％ |
| Comparative example 3 | 87.9％ |
The purity of the crocin obtained in each of examples and comparative examples was measured, and the results are shown in Table 2. As can be seen from Table 2, the purity of the crocin prepared in examples 1 to 4 is significantly higher than that of comparative examples 1 to 3, because the crocin is selectively adsorbed and extracted by using the molecular imprinting polymer microsphere technique in the invention, the specificity is good, and the purity of the finally extracted crocin is high.
In the embodiments 1-4, the saffron is extracted by utilizing the extraction process of the saffron, and then the saffron is selectively adsorbed by combining the chromatographic column filled with the saffron molecular engram polymer microsphere, so that the finally collected saffron glycoside has high extraction rate and good purity, and the saffron glycoside molecular engram polymer microsphere can be reused, thereby saving the cost and resources.
The number of equipment and the scale of processing described herein are intended to simplify the description of the present invention. Applications, modifications and variations of the present invention will be readily apparent to those skilled in the art.
Although embodiments of the present invention have been disclosed above, it is not limited to the details and embodiments shown and described, it is well suited to various fields of use for which the invention would be readily apparent to those skilled in the art, and accordingly, the invention is not limited to the specific details and illustrations shown and described herein, without departing from the general concepts defined in the claims and their equivalents.
Claims (4)
1. The extraction process of the crocin is characterized by mainly comprising the following steps of: grinding stigma croci Sativi, adding extraction solvent, extracting in a microwave extraction tank, collecting extractive solution, purifying and adsorbing with chromatography column filled with molecular engram polymer microsphere of stigma croci Sativi glycoside, collecting eluate, concentrating, and drying to obtain stigma croci Sativi glycoside;
the preparation method of the crocin molecularly imprinted polymer microsphere comprises the following steps:
step one, feCl 3 ·6H 2 Dissolving O in citric acid solution, adding glycol as dispersing agent, heating at 65-80 ℃ for 1-5h to form ferric oxide sol, mixing the ferric oxide sol with silicon dioxide sol to obtain mixed sol, adding urea and formaldehyde, heating, filtering, drying, calcining at 500-1000 ℃ for 5-8h to obtain magnetic silica gel microspheres, wherein the molar ratio of the silicon dioxide sol to the ferric oxide sol to the urea to the formaldehyde is (20-40): 1: (5-10): (8-15);
step two, the molar ratio is (1-2): 1 and itaconic acid are mixed, heated for 30-90 min at 50-100 ℃ to prepare choline chloride-itaconic acid, and crocin and choline chloride-itaconic acid are mixed according to a mole ratio of 1: (5-10) dissolving in ethanol solution, adding azodiisobutyronitrile and ethylene glycol dimethacrylate, and 1-butyl-3-methylimidazole tetrafluoroborate, and introducing nitrogen to prepare a mixed solution, wherein the mol ratio of the azodiisobutyronitrile to the ethylene glycol dimethacrylate, the 1-butyl-3-methylimidazole tetrafluoroborate to the choline chloride-itaconic acid is (1-3): (4-6): (10-15): 1;
immersing the magnetic silica gel microspheres prepared in the first step into the mixed solution prepared in the second step, performing ultrasonic dispersion at 60 ℃ until the microspheres are completely polymerized, and taking out the microspheres to wash with methanol and acetic acid solution with the volume ratio of 9:1 to prepare the saffron glycoside molecularly imprinted polymer microspheres;
the average particle diameter of the saffron glucoside molecularly imprinted polymer microsphere is 30-100 mu m.
2. The process according to claim 1, wherein the calcination temperature in the first step is 800 ℃ and the calcination time is 6 hours.
3. The extraction process of crocin according to claim 1, wherein the specific steps of purifying and adsorbing the extract are as follows:
step a, filling the saffron glucoside molecularly imprinted polymer microspheres into a chromatographic column, and prepressing for 8-10h by using petroleum ether as a mobile phase;
b, injecting the extract liquid obtained after saffron extraction into a chromatographic column for purification and adsorption, wherein the eluent is petroleum ether, the flow rate is 0.5-1 ml/min, collecting the eluent, and measuring the absorbance;
and c, replacing ethanol as eluent to wash the chromatographic column, collecting eluent, concentrating and drying to finally obtain the crocin.
4. The process according to claim 1, wherein the extraction solvent is one or more of water, ethanol and propylene glycol.
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