CN101530444A - Soft capsules of volatile oil of chrysanthemum - Google Patents
Soft capsules of volatile oil of chrysanthemum Download PDFInfo
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- CN101530444A CN101530444A CN200810019638A CN200810019638A CN101530444A CN 101530444 A CN101530444 A CN 101530444A CN 200810019638 A CN200810019638 A CN 200810019638A CN 200810019638 A CN200810019638 A CN 200810019638A CN 101530444 A CN101530444 A CN 101530444A
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Abstract
The invention relates to a method for extracting volatile oil from chrysanthemum and preparing soft capsules of volatile oil of chrysanthemum. The method is characterized in that the preparation method comprises the following steps: (1) the extracting technique of volatile oil is as follows: picked fresh chrysanthemum is dried and crushed after microwave heating; chrysanthemum powder is infused in saturated sodium chloride solution and is placed for 8 to 15 hours after stirring; an upper opening of a container tank is communicated with an air inlet of a volatile oil extractor; the container tank is heated and hold micro-boiling for 10 to 15 hours and the volatile oil is extracted; and the mixture solution of the extracted volatile oil is dehydrated, normal hexane is volatilized in natural room temperature with indoor ventilation and light shielding so as to obtain pale yellow volatile oil; and (2) the technique process for preparing the soft capsules of volatile oil of chrysanthemum comprises the following steps: firstly colloidal emulsion is prepared; and then a dropping machine is adopted to produce soft capsule. The technique is simple and convenient and is easy to operate, and has high extraction rate, little pollution and high purity. The soft capsule prepared by volatile oil products of chrysanthemum is convenient for eating and further improves the utilization value of chrysanthemum.
Description
Technical field:
The present invention relates to a kind ofly from Chinese herbal medicine, extract active ingredient and make soft capsule, especially a kind ofly from Flos Chrysanthemi, extract volatile oil and make soft capsules of volatile oil of chrysanthemum.
Background technology:
The development and utilization of natural resources of Chinese medicinal materials in recent years is China and even worldwide focus, and especially medicine food dual purpose plant has obtained very big development aspect the utilizing of health food and medicine.Flos Chrysanthemi can be used as medicine, and also can be used for making tea drinking and being widely used.Volatile oil in the Flos Chrysanthemi has heat-clearing and toxic substances removing, blood pressure lowering, effect such as antibacterial, but has not yet to see the report that the relevant volatile oil component that extracts in the processing Flos Chrysanthemi is made the finished product aspect.
If adopt the volatile oil in the traditional way of distillation extraction Flos Chrysanthemi of prior art, have some problems through test: the volatile oil that relative density is big is easy to sink in the water layer, even is sunken to the lower curtate of accepter; The volatile oil that distills out can be attached on the inwall of determinator; These situations all can not be collected in volatile oil in the oil reservoir fully, cause waste resource and extraction yield low, and cause environmental pollution.
Summary of the invention
The objective of the invention is to overcome traditional way of distillation and extract the situation of volatile oil yield waste on the low side, traditional extraction conditions is carried out process optimization, make the extraction ratio that can not only improve Flos Chrysanthemi volatile oil, and pollute little, purity is high.
Another object of the present invention provides a kind of process of the volatile oil that extracts being made soft capsule.
For achieving the above object, the technical solution adopted in the present invention is: this Flos Chrysanthemi volatile oil capsule, its preparation method comprises the steps:
(1), volatile oil extraction process:
(1), the bright Flos Chrysanthemi that will pluck, after the Preliminary screening roguing, with frequency is that the microwave deactivation of enzyme machine of 2450 ± 50MHz carries out 30-50 microwave deactivation of enzyme second, Flos Chrysanthemi after completing enters drying room and carries out forced air drying, blast temperature is 60-70 ℃, be 3-6 hour drying time, and exsiccant Flos Chrysanthemi was through pulverizing 80 orders-100 mesh sieve;
(2), preparation saturated nacl aqueous solution its weight be Flos Chrysanthemi powder weight 12-15 doubly;
(3), the dry Flos Chrysanthemi powder is put in the saturated nacl aqueous solution, and throw in some beades in the container jar of dry Flos Chrysanthemi powder and saturated nacl aqueous solution, placement is 8-15 hour after fully stirring;
(4), the air inlet of the suitable for reading of container jar and volatile oil extractor body is connected, at the condensation chamber of the volatile oil extractor water that adds suitable for reading, make water be full of that volatile oil preserves the chamber and when overfall flows into the container jar till; Then add 1-3ml ratio adding normal hexane in 100g Flos Chrysanthemi dry powder from the suitable for reading of condensation chamber;
(5), container tank is the extraction pot of band heating jacket, and container tank is heated to pot liquid boiling, boiling back homoiothermic kept pot liquid little 10-15 of boiling hour, extracted volatile oil;
(6), stop heating after, placed 0.5-2 hour, open the switch of volatile oil extractor body lower end, water is slowly emitted collection volatile oil;
(7), in collected volatile oil mixed liquor, add anhydrous sodium sulfate dehydration, the ratio of the anhydrous sodium sulfate of adding and volatile oil mixed liquor is: add the 1-2g anhydrous sodium sulfate in the volatile oil mixed liquor that extracts by 100g Flos Chrysanthemi dry powder; Volatile oil mixed liquor after dehydration places room ventilation lucifuge place to place 15-24 hour, and normal hexane is removed in volatilization in natural room temperature, obtains faint yellow volatile oil;
(2), the technological process of soft capsules of volatile oil of chrysanthemum preparation
(1), the preparation of colloidal emulsion
The component of colloidal emulsion and weight percent content are: gelatin 30-60%, glycerol 5-25%, surfactant 0.1-10%, antibacterial 0-1%, oils and fats 0.1-10%, water surplus;
(2) preparation method of colloidal emulsion comprises the steps: at first surfactant, oils and fats and the water of above-mentioned content are prepared into Emulsion; After gelatin, glycerol, antibacterial are added to the water, be heated to 60-80 ℃, stir, add above-mentioned Emulsion, stir, the degassing, colloidal emulsion.
(3), dropping preparation method prepares soft capsules of volatile oil of chrysanthemum
Adopt and drip system machine production soft capsule, Flos Chrysanthemi volatile oil is added in the material bin; Colloidal emulsion adds in the rubber cement bucket, and maintains the temperature in the 50-70 ℃ of scope; Contain in the soft capsule device and put into liquid paraffin, according to content of dispersion 0.25-0.28ml in each soft gelatin capsule, regulate Flos Chrysanthemi volatile oil discharging opening and gum exudation mouth, colloidal emulsion drips to above the liquid paraffin earlier and launches, volatile oil drops on the just unfolded gelatin surface immediately, because the principle of acceleration of gravity, rubber continues to descend, rubber is sealed fully, oil plant just is wrapped in the rubber the inside, adds surface tension effects, makes rubber become spheroidal, because temperature constantly descends, being frozen into soft capsule gradually, is 20～30 ℃ of cold air dryings with the soft gelatin capsule that makes in room temperature, passes through with the residual paraffin oil of 95% ethanol flush away soft capsule outer surface again, then place 30～35 ℃ of baking ovens interior 12-15 hour, and promptly got soft capsule.
Described a kind of Flos Chrysanthemi volatile oil capsule, it is characterized in that: according to drug effect and intend clinical consumption, design every seed lac ball and contain volatile oil 0.25-0.28ml, less because of measuring, available disperse medium dilution is made per 1 and is contained 0.4-0.6ml content soft gelatin capsule approximately, this soft capsule selects for use vegetable oil as disperse medium, its ratio volatile oil: salad oil is 1:1.
The present invention's beneficial effect compared with prior art:
The present invention has overcome the situation that the traditional way of distillation is extracted the waste on the low side of volatile oil yield, and this extraction process is simple and easy to do, and by demonstration test, extraction ratio is 0.51-0.58% under this extraction process condition, and pollute little, purity is high.With the soft capsule that the Flos Chrysanthemi volatile oil product is made, instant has further improved the value of Flos Chrysanthemi.
Description of drawings:
Fig. 1 extracts schematic diagram for the present invention.
Among the figure:
1. condensation chamber, 2. volatile oil preserves the chamber, 3. switch, 4. container tank, 5. volatile oil extractor body
The specific embodiment:
Describe the present invention in detail below in conjunction with accompanying drawing:
Preparation method of the present invention comprises the steps:
(1), volatile oil extraction process:
(1), the foreign horse Flos Chrysanthemi Flos Chrysanthemi flower that will pluck, after the Preliminary screening roguing, with frequency is that the microwave deactivation of enzyme machine of 2450 ± 50MHz carries out 40 seconds microwave deactivation of enzyme, Flos Chrysanthemi after completing enters drying room and carries out forced air drying, blast temperature is 65 ℃, be 5 hours drying time, and exsiccant Flos Chrysanthemi was through pulverizing 90 mesh sieves;
(2), preparation saturated nacl aqueous solution its weight is 12.5 times of Flos Chrysanthemi powder weight;
(3), the dry Flos Chrysanthemi powder is put in the saturated nacl aqueous solution, and throw in some beades in the container jar 4 of dry Flos Chrysanthemi powder and saturated nacl aqueous solution, placement is 10 hours after fully stirring;
(4), the air inlet of the suitable for reading of container jar 4 and volatile oil extractor body 5 is connected, at condensation chamber 1 water that adds suitable for reading of volatile oil extractor, make water be full of that volatile oil preserves chamber 5 and when overfall 6 flows into container jars 4 till; Then add 2.2ml ratio adding normal hexane in 100g Flos Chrysanthemi dry powder from the suitable for reading of condensation chamber 1;
(5), container tank 4 is the extraction pot of band heating jacket, and container tank 4 is heated to the pot liquid boiling, boiling back homoiothermic makes pot liquid keep little boiling 12 hours, extracts volatile oil; It extracts work process: the water vapour that container tank 4 heating backs produce, rise to condensation chamber 1 rapidly by volatile oil extractor body 5 air inlets, preserve chamber 2 through condensation chamber 1 liquid coolant of coming out through volatile oil, under the effect of normal hexane, add the light specific gravity of oil ratio water, make volatile oil in the liquid coolant rest on volatile oil and preserve chamber 2, and the water of separating in the liquid coolant flows in the container tank 4 through overfall 6, reciprocation cycle was extracted volatile oil 12 hours continuously like this;
(6), stop heating after, placed 1.5 hours, open the switch 3 of volatile oil extractor body 5 lower ends, water is slowly emitted collection volatile oil;
(7), in collected volatile oil mixed liquor, add anhydrous sodium sulfate dehydration, the ratio of the anhydrous sodium sulfate of adding and volatile oil mixed liquor is: add the 1-2g anhydrous sodium sulfate in the volatile oil mixed liquor that extracts by 100g Flos Chrysanthemi dry powder; Volatile oil mixed liquor after dehydration places room ventilation lucifuge place to place 20 hours, and normal hexane is removed in volatilization in natural room temperature, obtains faint yellow volatile oil;
(2), the technological process of soft capsules of volatile oil of chrysanthemum preparation
(1), the selection of disperse medium and adjuvant
According to drug effect and intend clinical consumption, design every seed lac ball and contain volatile oil 0.270ml, less because of measuring, available disperse medium dilution is made per 1 and is contained 0.53ml content soft gelatin capsule approximately, soft capsule selects for use vegetable oil as disperse medium, and is nontoxic, is easy to intestinal absorption, this product raw material is a volatile oil, room temperature is liquid down, does not exist with medium and mixes back thixotroping value height problem, according to the similar principle that mixes, it is feasible to select vegetable oil to make disperse medium, is dispersant so select salad oil of high quality and at a reasonable price for use.Its ratio volatile oil: salad oil (v/v) is 1:1.
(2), the preparation of colloidal emulsion
The component of colloidal emulsion and weight percent content are: gelatin 50%, glycerol 15%, surfactant 3%, antibacterial 0.5%, oils and fats 3%, water surplus;
(3) preparation method of colloidal emulsion comprises the steps: at first surfactant, oils and fats and the water of above-mentioned content are prepared into Emulsion; After gelatin, glycerol, antibacterial are added to the water, be heated to 70 ℃, stir, add above-mentioned Emulsion, stir, the degassing, colloidal emulsion.
(4), dropping preparation method prepares soft capsules of volatile oil of chrysanthemum
Adopt and drip system machine production soft capsule, Flos Chrysanthemi volatile oil is added in the material bin; Colloidal emulsion adds in the rubber cement bucket, and maintains the temperature in 60 ℃ of scopes; Contain in the soft capsule device and put into liquid paraffin, according to content of dispersion 0.270ml in each soft gelatin capsule, regulate Flos Chrysanthemi volatile oil discharging opening and gum exudation mouth, colloidal emulsion drips to above the liquid paraffin earlier and launches, volatile oil drops on the just unfolded gelatin surface immediately, because the principle of acceleration of gravity, rubber continues to descend, rubber is sealed fully, oil plant just is wrapped in the rubber the inside, adds surface tension effects, makes rubber become spheroidal, because temperature constantly descends, being frozen into soft capsule gradually, is 20～30 ℃ of cold air dryings with the soft gelatin capsule that makes in room temperature, passes through with the residual paraffin oil of 95% ethanol flush away soft capsule outer surface again, then place 32 ℃ of baking ovens interior 12 hours, and promptly got soft capsule.
(5), check and pack soft capsule
The soft capsule that scrutiny will be taken out from baking oven chooses underproof, and qualified products are packed warehouse-in.
Analyzing the mice consumption according to the zoopery result is 0.04ml/kgd, is 4.4ul/kgd with the consumption conversion for people's consumption, and adult's consumption is 0.264ml/d (pressing the 60kg body weight calculates), promptly takes a capsules for each person every day and gets final product.
Claims (2)
1, a kind of Flos Chrysanthemi volatile oil capsule, it is characterized in that: its preparation method comprises the steps:
(1), the bright Flos Chrysanthemi that will pluck, after the Preliminary screening roguing, with frequency is that the microwave deactivation of enzyme machine of 2450 ± 50MHz carries out 30-50 microwave deactivation of enzyme second, Flos Chrysanthemi after completing enters drying room and carries out forced air drying, blast temperature is 60-70 ℃, be 3-6 hour drying time, and exsiccant Flos Chrysanthemi was through pulverizing 80 orders-100 mesh sieve;
(2), preparation saturated nacl aqueous solution its weight be Flos Chrysanthemi powder weight 12-15 doubly;
(3), the dry Flos Chrysanthemi powder is put in the saturated nacl aqueous solution, and throw in some beades in the container jar (4) of dry Flos Chrysanthemi powder and saturated nacl aqueous solution, placement is 8-15 hour after fully stirring;
(4), the air inlet of the suitable for reading of container jar (4) with volatile oil extractor body (5) is connected, at condensation chamber (1) water that adds suitable for reading of volatile oil extractor, make water be full of that volatile oil preserves chamber (5) and when overfall (6) flows into container jar (4) till; Then add 1-3ml ratio adding normal hexane in 100g Flos Chrysanthemi dry powder from the suitable for reading of condensation chamber (1);
(5), container tank (4) is the extraction pot of band heating jacket, and container tank (4) is heated to pot liquid boiling, boiling back homoiothermic kept pot liquid little 10-15 of boiling hour, extracted volatile oil;
(6), stop heating after, placed 0.5-2 hour, open the switch (3) of volatile oil extractor body (5) lower end, water is slowly emitted collection volatile oil;
(7), in collected volatile oil mixed liquor, add anhydrous sodium sulfate dehydration, the ratio of the anhydrous sodium sulfate of adding and volatile oil mixed liquor is: add the 1-2g anhydrous sodium sulfate in the volatile oil mixed liquor that extracts by 100g Flos Chrysanthemi dry powder; Volatile oil mixed liquor after dehydration places room ventilation lucifuge place to place 15-24 hour, and normal hexane is removed in volatilization in natural room temperature, obtains faint yellow volatile oil;
(2), the technological process of soft capsules of volatile oil of chrysanthemum preparation
(1), the preparation of colloidal emulsion
The component of colloidal emulsion and weight percent content are: gelatin 30-60%, glycerol 5-25%, surfactant 0.1-10%, antibacterial 0-1%, oils and fats 0.1-10%, water surplus;
(2) preparation method of colloidal emulsion comprises the steps: at first surfactant, oils and fats and the water of above-mentioned content are prepared into Emulsion; After gelatin, glycerol, antibacterial are added to the water, be heated to 60-80 ℃, stir, add above-mentioned Emulsion, stir, the degassing, colloidal emulsion.
(3), dropping preparation method prepares soft capsules of volatile oil of chrysanthemum
Adopt and drip system machine production soft capsule, Flos Chrysanthemi volatile oil is added in the material bin; Colloidal emulsion adds in the rubber cement bucket, and maintains the temperature in the 50-70 ℃ of scope; Contain in the soft capsule device and put into liquid paraffin, according to content of dispersion 0.25-0.28ml in each soft gelatin capsule, regulate Flos Chrysanthemi volatile oil discharging opening and gum exudation mouth, colloidal emulsion drips to above the liquid paraffin earlier and launches, volatile oil drops on the just unfolded gelatin surface immediately, because the principle of acceleration of gravity, rubber continues to descend, rubber is sealed fully, oil plant just is wrapped in the rubber the inside, adds surface tension effects, makes rubber become spheroidal, because temperature constantly descends, being frozen into soft capsule gradually, is 20～30 ℃ of cold air dryings with the soft gelatin capsule that makes in room temperature, passes through with the residual paraffin oil of 95% ethanol flush away soft capsule outer surface again, then place 30～35 ℃ of baking ovens interior 12-15 hour, and promptly got soft capsule.
2, a kind of Flos Chrysanthemi volatile oil capsule according to claim 1, it is characterized in that: according to drug effect and intend clinical consumption, design every seed lac ball and contain volatile oil 0.25-0.28ml, less because of measuring, available disperse medium dilution is made per 1 and is contained 0.4-0.6ml content soft gelatin capsule approximately, this soft capsule selects for use vegetable oil as disperse medium, its ratio volatile oil: salad oil is 1:1.
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| CN102415603A (en) * | 2011-11-08 | 2012-04-18 | 林利强 | Method for preparing dry chrysanthemum by using fresh chrysanthemum |
| CN101715855B (en) * | 2009-12-17 | 2012-04-25 | 安徽省庆元堂徽菊有限公司 | Process for manufacturing dry chrysanthemum |
| CN101703137B (en) * | 2009-11-17 | 2012-05-09 | 射阳县东茗菊花茶厂 | Milk chrysanthemum (chrysanthemum rice) tea and processing method thereof |
| CN104513707A (en) * | 2014-12-16 | 2015-04-15 | 四川农业大学 | Method for extracting chrysanthemum essential oil and the extracted essential oil |
| CN104560401A (en) * | 2014-12-26 | 2015-04-29 | 高俊丽 | Extraction method of calendula volatile oil |
| CN104611137A (en) * | 2015-01-16 | 2015-05-13 | 江汉大学 | Extraction method of chrysanthemum morifolium volatile oil |
| CN105606423A (en) * | 2016-02-26 | 2016-05-25 | 河南中烟工业有限责任公司 | Extracting device and extracting method for volatile and semivolatile components in sample |
| CN105964312A (en) * | 2010-07-22 | 2016-09-28 | 基因细胞生物系统有限公司 | Composite liquid cells |
| US10252261B2 (en) | 2012-11-27 | 2019-04-09 | Gencell Biosystems Ltd. | Handling liquid samples |
| CN109628223A (en) * | 2018-12-07 | 2019-04-16 | 东南大学 | A kind of preparation method of chrysanthemum essential oil |
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Cited By (14)
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| CN101703137B (en) * | 2009-11-17 | 2012-05-09 | 射阳县东茗菊花茶厂 | Milk chrysanthemum (chrysanthemum rice) tea and processing method thereof |
| CN101715855B (en) * | 2009-12-17 | 2012-04-25 | 安徽省庆元堂徽菊有限公司 | Process for manufacturing dry chrysanthemum |
| CN105964312A (en) * | 2010-07-22 | 2016-09-28 | 基因细胞生物系统有限公司 | Composite liquid cells |
| US10125389B2 (en) | 2010-07-22 | 2018-11-13 | Gencell Biosystems Limited | Composite liquid cells |
| CN102415603B (en) * | 2011-11-08 | 2014-02-19 | 林利强 | Method for preparing dry chrysanthemum by using fresh chrysanthemum |
| CN102415603A (en) * | 2011-11-08 | 2012-04-18 | 林利强 | Method for preparing dry chrysanthemum by using fresh chrysanthemum |
| US10252261B2 (en) | 2012-11-27 | 2019-04-09 | Gencell Biosystems Ltd. | Handling liquid samples |
| US10384187B2 (en) | 2014-02-10 | 2019-08-20 | Gencell Biosystems Ltd | Composite liquid cell (CLC) mediated nucleic acid library preparation device, and methods for using the same |
| CN104513707B (en) * | 2014-12-16 | 2017-07-28 | 四川农业大学 | A kind of extracting method of chrysanthemum essential oil and the essential oil of extraction |
| CN104513707A (en) * | 2014-12-16 | 2015-04-15 | 四川农业大学 | Method for extracting chrysanthemum essential oil and the extracted essential oil |
| CN104560401A (en) * | 2014-12-26 | 2015-04-29 | 高俊丽 | Extraction method of calendula volatile oil |
| CN104611137A (en) * | 2015-01-16 | 2015-05-13 | 江汉大学 | Extraction method of chrysanthemum morifolium volatile oil |
| CN105606423A (en) * | 2016-02-26 | 2016-05-25 | 河南中烟工业有限责任公司 | Extracting device and extracting method for volatile and semivolatile components in sample |
| CN109628223A (en) * | 2018-12-07 | 2019-04-16 | 东南大学 | A kind of preparation method of chrysanthemum essential oil |
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