CN106691953B - A cigarette containing rhizoma Sparganii extract - Google Patents

A cigarette containing rhizoma Sparganii extract Download PDF

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Publication number
CN106691953B
CN106691953B CN201611012342.0A CN201611012342A CN106691953B CN 106691953 B CN106691953 B CN 106691953B CN 201611012342 A CN201611012342 A CN 201611012342A CN 106691953 B CN106691953 B CN 106691953B
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rhizoma sparganii
extract
enzymolysis
weight
carrying
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CN106691953A (en
Inventor
余汉谋
肖海鸿
姜兴涛
王晓莉
吴新星
黄文烨
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Dongguan Boton Flavors & Fragrances Co ltd
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Dongguan Boton Flavors & Fragrances Co ltd
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    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K8/00Cosmetics or similar toiletry preparations
    • A61K8/18Cosmetics or similar toiletry preparations characterised by the composition
    • A61K8/96Cosmetics or similar toiletry preparations characterised by the composition containing materials, or derivatives thereof of undetermined constitution
    • A61K8/97Cosmetics or similar toiletry preparations characterised by the composition containing materials, or derivatives thereof of undetermined constitution from algae, fungi, lichens or plants; from derivatives thereof
    • AHUMAN NECESSITIES
    • A24TOBACCO; CIGARS; CIGARETTES; SIMULATED SMOKING DEVICES; SMOKERS' REQUISITES
    • A24BMANUFACTURE OR PREPARATION OF TOBACCO FOR SMOKING OR CHEWING; TOBACCO; SNUFF
    • A24B15/00Chemical features or treatment of tobacco; Tobacco substitutes, e.g. in liquid form
    • A24B15/18Treatment of tobacco products or tobacco substitutes
    • A24B15/28Treatment of tobacco products or tobacco substitutes by chemical substances
    • A24B15/30Treatment of tobacco products or tobacco substitutes by chemical substances by organic substances
    • A24B15/302Treatment of tobacco products or tobacco substitutes by chemical substances by organic substances by natural substances obtained from animals or plants
    • A24B15/303Plant extracts other than tobacco
    • AHUMAN NECESSITIES
    • A24TOBACCO; CIGARS; CIGARETTES; SIMULATED SMOKING DEVICES; SMOKERS' REQUISITES
    • A24BMANUFACTURE OR PREPARATION OF TOBACCO FOR SMOKING OR CHEWING; TOBACCO; SNUFF
    • A24B15/00Chemical features or treatment of tobacco; Tobacco substitutes, e.g. in liquid form
    • A24B15/18Treatment of tobacco products or tobacco substitutes
    • A24B15/28Treatment of tobacco products or tobacco substitutes by chemical substances
    • A24B15/30Treatment of tobacco products or tobacco substitutes by chemical substances by organic substances
    • A24B15/305Treatment of tobacco products or tobacco substitutes by chemical substances by organic substances of undetermined constitution characterised by their preparation
    • A24B15/307Treatment of tobacco products or tobacco substitutes by chemical substances by organic substances of undetermined constitution characterised by their preparation using microorganisms or enzymes as catalysts
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61QSPECIFIC USE OF COSMETICS OR SIMILAR TOILETRY PREPARATIONS
    • A61Q19/00Preparations for care of the skin
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61QSPECIFIC USE OF COSMETICS OR SIMILAR TOILETRY PREPARATIONS
    • A61Q19/00Preparations for care of the skin
    • A61Q19/08Anti-ageing preparations
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K2800/00Properties of cosmetic compositions or active ingredients thereof or formulation aids used therein and process related aspects
    • A61K2800/80Process related aspects concerning the preparation of the cosmetic composition or the storage or application thereof
    • A61K2800/805Corresponding aspects not provided for by any of codes A61K2800/81 - A61K2800/95

Abstract

The invention relates to the technical field of plant extraction processes and plant extract application, in particular to a method for extracting a rhizoma sparganii extract, a cigarette containing the rhizoma sparganii extract and essence cream, and the method for extracting the rhizoma sparganii extract is characterized by comprising the following steps of: the method comprises the following steps: pulverizing rhizoma Sparganii extract, adding into ethanol water solution for extraction, mixing filtrates, and concentrating under reduced pressure to obtain rhizoma Sparganii extract; centrifuging the rhizoma sparganii extracting solution, sequentially carrying out enzymolysis treatment twice on the centrifugate, heating after the enzymolysis is finished to obtain the rhizoma sparganii enzymolysis solution, carrying out column chromatography adsorption twice on the rhizoma sparganii enzymolysis solution, collecting water eluent, carrying out reduced pressure concentration and freeze drying on target eluent to obtain the rhizoma sparganii extract, adding the rhizoma sparganii extract into cigarettes, and having the effects of improving the smoke state, enriching the smoke fragrance, removing impurities, reducing the thorn and the like. After in vitro tests, the rhizoma sparganii extract is found to have good effects of scavenging free radicals and preserving moisture, and can also be applied to moisturizing and anti-aging cosmetics.

Description

A cigarette containing rhizoma Sparganii extract
Technical Field
The invention relates to the technical field of plant extraction processes and application of plant extracts, in particular to an extraction method of a rhizoma sparganii extract, and cigarettes and essence cream containing the rhizoma sparganii extract.
Background
Chinese land is large and has various plant varieties, and the compositions of the contained effective components have various characteristics, thereby providing rich resources for the development of the effective plant additive. The effective components of the plants can be extracted and separated by different methods, and the application of the effective components of the plants in different fields is explored, so that the economic value of the effective components of the plants is improved.
The rhizoma Sparganii is dried tuber of Sparganium stoloniferum Buch-ham. of Sparganium of Sparganiaceae. Collected in winter to spring of the next year, cleaned, peeled and dried in the sun. It was recorded in "Ben Cao Shi Yi" of Tang Dynasty, and was recorded in "Chinese pharmacopoeia" of Song Dynasty. Rhizoma Sparganii is neutral in nature and bitter in taste, and has effects of breaking blood and activating qi-flowing, resolving food stagnation and relieving pain when entering liver and spleen channels. Modern pharmacological research shows that the rhizoma sparganii has the effects of resisting tumor, resisting oxidation, easing pain, resisting inflammation, resisting blood coagulation, resisting platelet aggregation, resisting thrombus, resisting pulmonary fibrosis and the like, and is a common traditional Chinese medicine for promoting blood circulation and removing blood stasis. Research shows that the components related to pharmacological activity mainly include phenols, flavones, saponins and polysaccharides.
The common burreed rhizome is widely applied, reports and researches on the common burreed rhizome are numerous at present, but most of the common burreed rhizome is mixed with other medicinal materials for use, the extraction method of the common burreed rhizome is only limited to leaching or organic matter purification at present, the time is long, the extraction efficiency is low, the total method mainly aims at extracting flavone in the common burreed rhizome, and other components and application researches on the common burreed rhizome are few.
Disclosure of Invention
In order to overcome the defects and shortcomings in the prior art, the invention aims to provide the method for extracting the rhizoma sparganii extract, which is used for directly obtaining effective active substances from the rhizoma sparganii, and has the advantages of simple and easily-operated step process, high effective components of the obtained extract, good purity and wide applicable range.
The other purpose of the invention is to provide the rhizoma sparganii extract which has high content of effective components and good application effect.
The invention also aims to provide application of the rhizoma sparganii extract, which can be applied to the field of cigarette feeding, is beneficial to improving the smoking quality of cigarettes and can also be applied to the fields of moisture preservation and aging resistance of cosmetics.
8. Essence cream containing rhizoma sparganii extract
The purpose of the invention is realized by the following technical scheme:
a method for extracting rhizoma Sparganii extract comprises the following steps:
the method comprises the following steps: pulverizing rhizoma Sparganii extract in a weight part, adding into ethanol water solution, extracting for 1-3 times, adding 8a-10a weight parts of ethanol water solution each time, mixing filtrates, and concentrating under reduced pressure to obtain rhizoma Sparganii extract in a weight part;
step two: centrifuging the rhizoma sparganii extracting solution in part by weight, sequentially carrying out enzymolysis treatment on the centrifugate twice, wherein the enzymolysis temperature is 37 ℃, the time is 30-60min, and after the enzymolysis is finished, heating to 80-90 ℃ and keeping for 15-30min to obtain rhizoma sparganii enzymolysis liquid; enzymolysis helps to decompose starch, protein, pectin and other components which affect the activity effect.
Step three: and carrying out first column chromatography on the rhizoma sparganii enzymolysis liquid, collecting water eluent, carrying out secondary column chromatography adsorption, collecting water eluent, and carrying out reduced pressure concentration and freeze drying on target eluent to obtain the rhizoma sparganii extract. The column chromatography aims at decoloring, purifying and improving the content of active ingredients in the rhizoma sparganii extract.
Wherein the ethanol water solution in the first step has the mass fraction of 5-40% of ethanol.
Wherein, in the second step, 0.01a-0.03a parts by weight of complex enzyme is used for the first enzymolysis, and the complex enzyme comprises amylase, cellulase and pectinase according to the mass ratio: 3-5: 1-2: 1-2, mixing; the second enzymolysis is carried out by 0.005a-0.01a weight parts of protease. The biological enzyme used may be in solid or liquid form.
Wherein, in the third step, the first column chromatography filler is prepared by mixing kieselguhr and activated carbon particles according to the mass ratio of 1-2: 3-5, mixing; the second column chromatography packing is nonpolar macroporous resin. The model is but not limited to BS-65, X-5, HPD-100, HP20, D101, etc. The diatomite is combined with the activated carbon particles, so that the pigment in the rhizoma sparganii extract can be efficiently removed, and the effect is better than that of singly using one of the rhizoma sparganii extract. The nonpolar macroporous resin can further remove trace fat-soluble impurities in the rhizoma sparganii extract, and plays a role in impurity removal and purification.
A rhizoma Sparganii extract is obtained by the above method.
A cigarette containing rhizoma Sparganii extract is prepared by adding the rhizoma Sparganii extract 0.05-0.5 wt% of tobacco shred.
The application of the rhizoma sparganii extract in cosmetics comprises a substrate and the rhizoma sparganii extract, wherein the rhizoma sparganii extract accounts for 0.01-10% of the total weight of the cosmetics.
The cosmetic is in the form of solution, lotion or cream.
1. An essence cream containing rhizoma sparganii extract comprises the following components in percentage by mass:
phase A: cetostearyl alcohol 1-2%
Caprylic/capric triglyceride 4-5%
1 to 3 percent of squalane
2% of polydimethylsiloxane
2-5% of cyclopentasiloxane
Phase B: 3-5% of glycerin
1, 3-butanediol 1-3%
Allantoin 0.2%
0.1 to 0.3 percent of xanthan gum
Balance of water
And C phase: 0 to 0.2 percent of polyacrylamide
C13-14 isoparaffin 0-0.4%
Cinnamyl alcohol ether-70.2%
Phase D: rhizoma Sparganii extract 0.1-3%
Phase E: 0.1 to 0.2 percent of phenoxyethanol
0.1 to 0.2 percent of ethylhexyl glycerin,
the preparation method of the essence cream comprises the following steps: adding the phase A into an oil phase pot, and heating to 80 ℃; adding phase B into emulsifying pot, and heating to 80 deg.C; adding the phase A into the phase B for homogenizing for 2-3 minutes; adding phase C, homogenizing for 2-3 min; stirring, cooling to 30-40 deg.C, adding phase D and phase E, and making into essence cream containing rhizoma Sparganii extract.
The essence cream has the functions of moisturizing and removing free radicals, and has a remarkable effect in the anti-aging field.
The invention has the beneficial effects that: the preparation method of the rhizoma sparganii extract is safe, reliable, simple and efficient, firstly, crude extract is prepared through steps of extraction, concentration, enzymolysis and the like, and is further decolored through diatomite and active carbon particles, and then is subjected to secondary macroporous resin adsorption and purification, and the rhizoma sparganii extract is obtained through concentration and freeze drying. It can be added into cigarette to improve smoke state, enrich tobacco fragrance, remove impurities, and reduce irritation. After in vitro tests, the rhizoma sparganii extract is found to have good effects of scavenging free radicals and preserving moisture, and can also be applied to moisturizing and anti-aging cosmetics.
The method has the advantages of simple operation, easily obtained raw materials and good practical significance in industrial production.
Detailed Description
The present invention will be further described with reference to the following examples for facilitating understanding of those skilled in the art, and the description of the embodiments is not intended to limit the present invention.
Example 1
Weighing 100g of rhizoma sparganii extract, crushing, adding 800-1000g of ethanol aqueous solution (the mass fraction of ethanol is 35 percent), extracting for 2 times, combining filtrates, and concentrating under reduced pressure to obtain 100g of rhizoma sparganii extract; centrifuging the rhizoma sparganii extracting solution, adding 1.5g of complex enzyme into the centrifugate for enzymolysis, wherein the complex enzyme is amylase, cellulase and pectinase according to the mass ratio of 3: 1: 1 at 37 deg.C for 40 min. Heating to 85 ℃ after the first enzymolysis is finished, keeping the temperature for 20min, then cooling to 37 ℃, adding 0.8g of protease for enzymolysis for 30min, heating to 90 ℃ after the second enzymolysis is finished, keeping the temperature for 15min, and then cooling to normal temperature to obtain rhizoma sparganii enzymolysis liquid; and (2) enabling the rhizoma sparganii enzymolysis liquid to pass through a glass chromatographic column loaded with a mixture of kieselguhr and activated carbon particles, wherein the mixing ratio is 2: and 4, collecting deionized water eluent, carrying out X-5 macroporous resin adsorption for the second time, collecting the deionized water eluent, and carrying out reduced pressure concentration and freeze drying on the target eluent to obtain 11g of the rhizoma sparganii extract.
Example 2
Weighing 100g of rhizoma sparganii extract, crushing, adding 1000g of ethanol water solution (20% by mass of ethanol), extracting for 1 time, combining filtrates, and concentrating under reduced pressure to obtain 100g of rhizoma sparganii extract; centrifuging the rhizoma sparganii extracting solution, adding 2g of complex enzyme into the centrifugate for enzymolysis, wherein the complex enzyme is amylase, cellulase and pectinase according to a mass ratio of 5: 2: 1 at 37 deg.C for 50 min. After the first enzymolysis is finished, heating to 80 ℃ for 30min, then cooling to 37 ℃, adding 1g of protease for enzymolysis for 40min, after the second enzymolysis is finished, heating to 90 ℃ for 30min, and then cooling to normal temperature to obtain rhizoma sparganii enzymolysis liquid; and (2) enabling the rhizoma sparganii enzymolysis liquid to pass through a glass chromatographic column loaded with a mixture of kieselguhr and activated carbon particles, wherein the mixing ratio is 2: and 5, collecting deionized water eluent, carrying out D101 macroporous resin adsorption for the second time, collecting the deionized water eluent, and carrying out reduced pressure concentration and freeze drying on the target eluent to obtain 8.9g of the rhizoma sparganii extract.
Example 3
Weighing 100g of rhizoma sparganii extract, crushing, adding 900g of ethanol water solution (5% by mass of ethanol), extracting for 3 times, combining filtrates, and concentrating under reduced pressure to obtain 100g of rhizoma sparganii extract; centrifuging the rhizoma sparganii extracting solution, adding 3g of complex enzyme into the centrifugate for enzymolysis, wherein the complex enzyme is amylase, cellulase and pectinase according to a mass ratio of 5: 2: 1 at 37 deg.C for 60 min. Heating to 90 ℃ for 20min after the first enzymolysis is finished, then cooling to 37 ℃, adding 0.5g of protease for enzymolysis for 50min, heating to 85 ℃ for 15min after the second enzymolysis is finished, and then cooling to normal temperature to obtain rhizoma sparganii enzymolysis liquid; and (3) enabling the rhizoma sparganii enzymolysis liquid to pass through a glass chromatographic column loaded with a mixture of kieselguhr and activated carbon particles, wherein the mixing ratio is 1: and 5, collecting deionized water eluent, carrying out secondary HP20 macroporous resin adsorption, collecting deionized water eluent, carrying out reduced pressure concentration and freeze drying on the target eluent to obtain 9.7g of rhizoma sparganii extract.
The moisturizing activity and the effect of eliminating the radical activity of the trigone extract prepared by the preparation method of the above three examples were tested as follows.
Test 1: detection of skin moisturizing efficacy
10 healthy subjects were selected, with an average age of 31 years. The stratum corneum water content of subjects who were applied with the extracts of rhizoma sparganii at different concentrations was measured using a Corneometer825 from CK, germany.
Environmental conditions: the temperature and humidity of the environment are constant during the test period, the temperature is (25 +/-2) DEG C, and the relative humidity is 40-60%.
The smearing part is 4 and 8CM away from the elbow joint of the arm, the tested area is 3 × 3CM2, the time length is 60min, and the reading is expressed by Arbitrary Unit (A. U.).
The samples were diluted with deionized water to different concentrations and the deionized water solution was used as a blank control. The results are given in table 1 below.
TABLE 1 moisturizing ability test results
Figure 349987DEST_PATH_IMAGE001
As can be seen from Table 2, the trigone extract can achieve superior skin moisturizing capability, and the moisturizing capability is remarkably improved when the dosage is more than 1%. The rhizoma sparganii extract can be applied to moisturizing cosmetics and has a remarkable effect.
And (3) testing 2: detection of free radical scavenging Activity
The rhizoma sparganii extracts prepared in the examples 1, 2 and 3 are respectively dissolved in deionized water to prepare 0.5 mass percent solution, the activity of scavenging free radicals is measured by a DPPH free radical removal method, and VC (vitamin C) is used as a control sample.
The determination step comprises accurately transferring 2m L of the extractive solution into 10m L stoppered test tube, and adding 2m L DPPH ethanol solution (2 × 10)-4mol/L), mixing well, standing at room temperature, measuring absorbance A at wavelength of 517nm with spectrophotometer after 30min517(using ethanol as reference), and simultaneously measuring the absorbance A of the mixture of 2m L DPPH solution and 2m L ethanolCAnd absorbance A obtained by mixing 2m L extract with 2m L ethanol solution0. Triplicate determinations were made, the mean was taken, and the radical clearance was calculated according to the following formula:
radical clearance = (1- (a)517-A0)/AC)×100%。
The radical clearance rates of the trigone extract and VC obtained in the three examples were finally measured and are shown in table 2.
TABLE 2 radical scavenging rates of Sparganii extract and VC
Figure 226676DEST_PATH_IMAGE002
As can be seen from Table 2, the extract of Sparganii of the present invention all achieve radical scavenging effect, and is superior to VC of the same concentration at present. It is explained that the trigone extract of the present invention can be used in an anti-aging cosmetic.
The following will further describe the application of the rhizoma sparganii extract in the preferred embodiment of the invention in cosmetics with reference to specific embodiments.
Example 4: essence cream containing rhizoma sparganii extract
The rhizoma sparganii extract is used for preparing the skin care essence cream with the effects of moisturizing and resisting aging. Specific raw materials and contents are shown in table 3.
Table 3 materials and contents of essence cream
Figure 862188DEST_PATH_IMAGE004
The essence cream can be prepared by the following processes: adding the phase A into an oil phase pot, and heating to 80 ℃; adding phase B into emulsifying pot, and heating to 80 deg.C; adding the phase A into the phase B for homogenizing for 2-3 minutes; adding phase C, homogenizing for 2-3 min; stirring and cooling to 30-40 deg.C, adding phase D and phase E; the essence cream is subjected to skin moisturizing effect and free radical scavenging activity detection again, and the result shows that the essence cream has excellent moisturizing performance and anti-aging effect.
The following embodiments are provided to further explain the application of the rhizoma sparganii extract in the preferred embodiment of the invention in cigarettes.
Example 5: cigarette flavoring testing
The novel application of the rhizoma sparganii extract is to spray the rhizoma sparganii extract on the surface of tobacco leaves of flue-cured tobacco, wherein the spraying amount of the rhizoma sparganii extract accounts for 0.05-0.5% of the weight of sprayed tobacco shreds of the flue-cured tobacco.
Specific test tests: the rhizoma sparganii extract in the example 1 is diluted by deionized water and then used as an additive to be sprayed on the surface of the same middle-grade blank (without flavoring material) flue-cured tobacco shred, and the addition amounts are 0.05%, 0.1%, 0.2%, 0.5% and 0.8% of the weight of the tobacco shred respectively. The subsequent treatment is carried out according to the conventional cigarette process, namely after the tobacco flavor is sprayed, the cured tobacco shred is stored for 4 hours, and then the finished product of the cigarette is prepared through the procedures of shredding, shred drying, flavoring, shred storage, rolling and packaging. The above samples were subjected to a panel of 8 persons for a panel of 8 persons, and the overall sensory test results are shown in Table 4 below. Setting the internal quality of the blank sample to be 0, and correspondingly obtaining a positive score if the internal quality of the blank sample is improved (such as smooth smoke state, covering offensive odor, increasing fragrance amount and reducing stimulation) compared with the internal quality of the blank sample, wherein the improvement is better if the score is higher; the intrinsic quality is reduced relative to a blank sample (such as the smoke state sinks, the offensive odor increases, the fragrance amount is reduced, and the aftertaste is uncomfortable), the corresponding negative score is obtained, and the lower the negative score is, the worse the improvement is.
TABLE 4 Overall sensory test results
Figure 191538DEST_PATH_IMAGE006
The cigarette feeding and smoking evaluation experiment shows that the prepared rhizoma sparganii extract has a good perfuming effect, is coordinated with the cigarette fragrance, and can improve the smoke state, increase the fragrance amount, cover miscellaneous gases and reduce the irritation. The whole smoking quality of the flue-cured tobacco cigarette can be improved, and the application value is high.
The above-described embodiments are preferred implementations of the present invention, and the present invention may be implemented in other ways without departing from the spirit of the present invention.

Claims (4)

1. A cigarette containing a common burreed rhizome extract is characterized in that: the addition amount of the rhizoma sparganii extract is 0.05-0.5% of the weight of the cut tobacco, and the extraction method of the rhizoma sparganii extract comprises the following steps:
the method comprises the following steps: crushing 1 part by weight of rhizoma sparganii, adding the crushed rhizoma sparganii into an ethanol water solution for extraction for 1-3 times, adding 8-10 parts by weight of the ethanol water solution each time, combining filtrates, and concentrating under reduced pressure to obtain 1 part by weight of rhizoma sparganii extract;
step two: centrifuging 1 part by weight of the rhizoma sparganii extracting solution, sequentially carrying out enzymolysis treatment on the centrifugate twice, wherein the enzymolysis temperature is 37 ℃, the time is 30-60min, and after the enzymolysis is finished, heating to 80-90 ℃ and keeping for 15-30min to obtain rhizoma sparganii enzymolysis liquid;
step three: and carrying out first column chromatography on the rhizoma sparganii enzymolysis liquid, collecting water eluent, carrying out secondary column chromatography adsorption, collecting water eluent, and carrying out reduced pressure concentration and freeze drying on target eluent to obtain the rhizoma sparganii extract.
2. The cigarette containing the trigone extract according to claim 1, wherein the cigarette comprises: the mass fraction of the ethanol in the ethanol aqueous solution in the first step is 5-40%.
3. The cigarette containing the trigone extract according to claim 1, wherein the cigarette comprises: in the second step, 0.01-0.03 weight part of complex enzyme is used for the first enzymolysis, and the complex enzyme is prepared from amylase, cellulase and pectinase according to the mass ratio: 3-5: 1-2: 1-2, mixing; the second enzymolysis is carried out with 0.005-0.01 weight parts of protease.
4. The cigarette containing the trigone extract according to claim 1, wherein the cigarette comprises: in the third step, the first column chromatography filler is prepared from diatomite and activated carbon particles according to the mass ratio of 1-2: 3-5, mixing; the second column chromatography packing is nonpolar macroporous resin.
CN201611012342.0A 2016-11-17 2016-11-17 A cigarette containing rhizoma Sparganii extract Withdrawn - After Issue CN106691953B (en)

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中药三棱化学成分研究;袁涛;《中国优秀硕士学位论文全文数据库》;中国学术期刊(光盘版)电子杂志社;20170115(第01期);32-35 *

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