CN103462854B - Tire chrysanthemum hydrosol and preparation method thereof - Google Patents
Tire chrysanthemum hydrosol and preparation method thereof Download PDFInfo
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- CN103462854B CN103462854B CN201310444420.4A CN201310444420A CN103462854B CN 103462854 B CN103462854 B CN 103462854B CN 201310444420 A CN201310444420 A CN 201310444420A CN 103462854 B CN103462854 B CN 103462854B
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Abstract
The invention provides a kind of tire chrysanthemum hydrosol and preparation method thereof, pretreatment that preparation method comprises the steps: (1); (2) feed intake, infiltrate: tire chrysanthemum 50 ~ 100kg step 1 dried in the shade drops in distillating still, add 150 ~ 300kg deionized water to soak, be interrupted in immersion process and carry out low rate mixing, opened every 10-20 minute and once stir, mixing speed 10-15 rev/min, mixing time 1-2 minute; (3) ultrasonic Treatment; (4) distill; (5) clarify; (6) filter at low temperature: amalgamation liquid step 5 obtained preserves 24-48h under 2-3 DEG C of cryogenic conditions, then the filter plant pressure filtration using aperture 1-2 micron.The present invention is applied to tire chrysanthemum in the middle of cosmetics initiatively, and the tire chrysanthemum hydrosol obtained by it has fragrant tire chrysanthemum fragrance, steady quality not easily separates out precipitate, also has replenishing water and preserving moisture, skin maintenance effect simultaneously.
Description
Technical field
The invention belongs to cosmetic technical field, particularly a kind of tire chrysanthemum hydrosol and preparation method thereof.
Background technology
Tire chrysanthemum is also known as Flos Chrysanthemi, and also name little Tang Huang, chryanthemum parthenium, ancient times makes tribute.With the chrysanthemum scented tea of tire chrysanthemum bubble, taste is pure, strong, golden yellow color, has the delicate fragrance of nectar, and bubble does not fall apart for a long time.Record according to the traditional Chinese medical science, tire chrysanthemum, cold nature, acrid in the mouth sweetness and bitterness, can dispelling wind and heat pathogens, suppressing the hyperactive liver improving eyesight, heat-clearing and toxic substances removing, have that the spring warmly dries, summer summer-heat quenches one's thirst, autumn days separate dry, the winter relieves inflammation or internal heat, skin maintenance, refresh oneself, strengthen the effect such as vitality, slow down aging.But tire chrysanthemum often uses as a kind of tea by people, not yet find tire chrysanthemum to be applied in cosmetics, also have no pertinent literature report.
Hydrosol, also known as crystal's oil, a kind of cosmetics in recent years risen on the market, common as Camellia sinensis hydrosol, lavandula angustifolia hydrosol, MEIGUI CHUNLU, jasmine hydrosol, Flos Matricariae chamomillae hydrosol, fan repeatedly hydrosol, Fructus Citri Limoniae hydrosol, Herba Menthae hydrosol, orange blossom hydrosol etc., because it contains water-soluble substances (as tannin and flavonoid) and the denier quintessence oil of plant origin, nurse one's health helpful to whitening and skin-protecting, health.But the hydrosol on sale on the market vinasse therefrom separated when being mostly way of distillation extraction quintessence oil, and the skin protection of containing in flowers is worth quintessence oil that is high, that distribute pleasurable fragrance and is separated, the hydrosol that therefore prepared by traditional method has taste slightly acid, mostly without herbal delicate fragrance, working substance content also on the low side, the defect that is difficult to the skin effect of performance Feature flowers.
Summary of the invention
For making up the deficiencies in the prior art, the present invention is applied to tire chrysanthemum in the middle of cosmetics initiatively, a kind of preparation method of tire chrysanthemum hydrosol is provided, tire chrysanthemum hydrosol obtained by it has fragrant tire chrysanthemum fragrance, steady quality not easily separates out precipitate, also has replenishing water and preserving moisture, skin maintenance effect simultaneously.
To achieve the object of the present invention, adopt technical scheme as follows:
A preparation method for tire chrysanthemum hydrosol, comprises the steps:
(1) pretreatment: tire chrysanthemum flower is spread out in indoor and dries in the shade;
(2) feed intake, infiltrate: tire chrysanthemum 50 ~ 100kg step 1 dried in the shade drops in distillating still, add 150 ~ 300kg deionized water to soak, be interrupted in immersion process and carry out low rate mixing, opened every 10-20 minute and once stir, mixing speed 10-15 rev/min, mixing time 1-2 minute; (tire chrysanthemum flower more fully being soaked by being interrupted low rate mixing)
(3) ultrasonic Treatment: mixing speed controlled at 10-15 rev/min, opens the electric heater unit of distillating still, and heating material in distillating still is warming up to 85-90 DEG C; Frequency is adopted to be the ultrasonic Treatment 10-15 minute of 20kHZ;
(4) distill: after ultrasonic Treatment, heating material in distillating still is warmed up to 100 DEG C, opens the condenser of distillating still, and the cooling water that circulates within the condenser, start to collect distillate;
(5) clarify: the distillate of collection is left standstill 12-24 hour, extract the supernatant, turbid for bottom liquid is filtered simultaneously, filtrate and the supernatant are merged;
(6) filter at low temperature: amalgamation liquid step 5 obtained preserves 24-48h under 2-3 DEG C of cryogenic conditions, then the filter plant pressure filtration using aperture 1-2 micron.
Preferably, described preparation method also has step 7, and step 7 is: filter to step 6 in the filtrate of gained and add antiseptic, and its addition of described antiseptic is 0.3 ~ 0.5% of filtrate quality.
Preferably, described antiseptic is 1, the 2-hexanediol and 1,2-ethohexadiol that mix according to the mass ratio of 1:1-1:3.The tire chrysanthemum hydrosol that preparation method of the present invention obtains contains abundant nutritional labeling, will go bad very soon if not anticorrosion, affects product shelf phase and consumer's safety in utilization.The present invention preferably adopts 1,2 hexanediol and 1, and 2 ethohexadiols are antiseptic according to the mixture that special ratios forms, and can reach gentle antiseptical effect.1,2 hexanediol and 1,2 ethohexadiols itself are all polyhydric alcohol wetting agents, moisturizing and not Diazolidinyl Urea, and to skin without any stimulation, and the two also has collaborative antiseptic effect according to special ratios is composite, better can play the preservative efficacy of polyhydric alcohol.
Further, in step 5, the turbid liquid of bottom adopts 400-1000 object filter cloth to filter.
Further, in step 4, the gathering speed of distillate is controlled at 40-50kg/ hour, the persistent period that step 4 carries out distilling preferably controls at 3-4 hour, by the control to distillate gathering speed, be conducive to fully extracting the effective ingredient in tire chrysanthemum, the tire chrysanthemum hydrosol of distillation gained is about 100-250kg.The control of distillate gathering speed controls by following two aspects usually: the evaporation rate on the one hand by regulating the heating power of distillating still heater to control distillating still inner tube of a tyre chrysanthemum soak, concrete as, control, for 30kw, to collect distillate stage control at 40-45kw in distillation at heat temperature raising stepwise heating rating of set; Gathering speed on the other hand by regulating the liquid stream size of distillate drain pipe (those skilled in the art often regulate the liquid stream size of distillate drain pipe by being applied in linear flow gauge to realize) to regulate distillate, wherein the distillate distilled out is flowed back in distillating still by overflow pipe more.
Further, the tire chrysanthemum deionized water dried in the shade in step 2 soaks 1-2 hour.
The tire chrysanthemum hydrosol that second aspect present invention provides a kind of preparation method by mentioned earlier obtained.
Compared with prior art, technical scheme provided by the invention has following beneficial effect:
(1) what the present invention was initiative is applied in skin care item by tire chrysanthemum, not yet finds to adopt tire chrysanthemum to prepare the report of tire chrysanthemum hydrosol.Technical scheme of the present invention is that the application of tire chrysanthemum in skin care item provides a kind of effective way.
(2) in traditional hydrosol preparation technology, in distillating still, usually add salt to reduce the dissolubility of quintessence oil in distillate, improve the oil yield that quintessence oil is produced.Preparation method of the present invention has given up this step, remains distinctive derived essential oil in tire chrysanthemum flower to greatest extent.What the derived essential oil of tire chrysanthemum had dispels the wind and local irritant effect, can play the excellent results of heat clearing away toxin expelling; The pleasant fragrance that the derived essential oil of tire chrysanthemum is exclusive in addition, gives the result of use that product is better.
(3) preparation method of the present invention, adopts ultrasound wave to process before it is distilled, greatly facilitates extraction efficiency, increase the dissolution rate of tire chrysanthemum active component.The cavitation effect that ultrasonic Treatment is brought, can make tire Flos Chrysanthemi grass cell break because of the running quickly routed of generation cavitation bubble instantaneous in aqueous solution, make aqueous solution penetrate into cell interior, improve the extraction ratio of active substance in flowers.In addition, the present invention also carries out stand at low temperature and freezing and filtering to distillate, makes the macromolecular substances in distillate accelerate Precipitation, the microscopic precipitate filtering that the high-accuracy filter finally by 1-2 micron will be separated out under low temperature.Through the tire chrysanthemum hydrosol that this PROCESS FOR TREATMENT is crossed, within the shelf-life, do not have the phenomenon that visible foreign is separated out.Because of its complicated component of distillate collected, comprise the multiple macromolecular substances such as vegetable protein, tannin, vegetable polysaccharides.If do not processed the tire chrysanthemum hydrosol collected, after placing a period of time, macromolecular substances will be separated out gradually and be formed precipitation, have a strong impact on consumer and use.In traditional hydrosol preparation technology, often do not have filter operation, or only carry out room temperature filtration to distillate, hydrosol obtained like this, often appears in the shelf-life phenomenon just having visible foreign to separate out.
(4) its processing procedure of preparation method of the present invention merged immersion, ultrasonic, distillation, leave standstill filter, the multiple process means such as cryopreservation and filter at low temperature, adopt the treatment conditions of special parameter to prepare tire chrysanthemum hydrosol simultaneously, obtained tire chrysanthemum hydrosol contains abundant derived essential oil and other water-soluble active ingredients, obtained tire chrysanthemum hydrosol fragrance is pure, there is the tire chrysanthemum fragrance of fragrance, steady quality, not easily separate out precipitate, appearance transparent is clarified, and also has effect of replenishing water and preserving moisture, heat-clearing and toxic substances removing, skin maintenance simultaneously.
(5) the tire chrysanthemum hydrosol that the present invention obtains meets " cosmetics health specification " requirement completely, and meet sanitary index as shown in table 1 below, physical and chemical parameter and sense organ meet the requirements described in following table 2.
Table 1 sanitary index
Table 2 sense organ, physical and chemical index
(6) the tire chrysanthemum hydrosol zest obtained by is little, has no side effect.
Detailed description of the invention
Below in conjunction with embodiment, technical scheme of the present invention is described.
Embodiment 1(prepares tire chrysanthemum hydrosol by method of the present invention)
A kind of tire chrysanthemum hydrosol, preparation method preparation in accordance with the following steps:
(1) pretreatment: the tire chrysanthemum flower plucked tire chrysanthemum planting base is spread out in indoor and dried in the shade;
(2) feed intake, infiltrate: tire chrysanthemum 100kg step 1 dried in the shade drops in distillating still, add 300kg deionized water to soak, soak time is 1 hour, be interrupted in immersion process and carry out low rate mixing, opened every 15 minutes and once stir, mixing speed 10-15 rev/min, each mixing time is 1-2 minute;
(3) ultrasonic Treatment: first mixing speed is controlled, at 10-15 rev/min, then to open heater, heating material in distillating still is warming up to 90 DEG C; Frequency is adopted to be the ultrasonic Treatment 10 minutes of 20kHZ;
(4) distill: after ultrasonic Treatment, material in distillating still is heated to 100 DEG C, open the condenser of distillating still, and the cooling water that circulates within the condenser, start to collect distillate, what in still-process, adjust distillate distillates speed, makes the gathering speed of distillate control at 50kg/ hour, terminates distillation after 4 hours;
(5) clarify: the distillate collected is left standstill 24 hours, extracts the supernatant, turbid for bottom liquid 400 order filter clothes are filtered simultaneously, filtrate and the supernatant are merged;
(6) filter at low temperature: the distillate of clarification step 5 obtained preserves 24h under 2-3 DEG C of cryogenic conditions, then use the filter plant pressure filtration of aperture 1-2 micron.
(7) anticorrosion: to filter to step 6 in the filtrate of gained and add antiseptic, its addition of antiseptic is 0.4% of filtrate quality, and antiseptic is 1,2-hexanediol and 1, the 2-ethohexadiol of mass ratio 1:2.
(8) filling and package: according to packing specification in dust proof workshop fill, treats that end product quality after the assay was approved, and product good for fill is carried out labeling, stamp, vanning, packing, warehouse-in.
The tire chrysanthemum hydrosol that embodiment 1 obtains is through quality testing, and its microbiological indicator meets all standard above shown in table 1; Physical and chemical index assay and sense organ meet the requirements of table 2.Obtained tire chrysanthemum hydrosol fragrance is pure, and have the tire chrysanthemum fragrance of fragrance, steady quality, places and also do not separate out precipitate in 3 years, and appearance transparent is clarified.
Embodiment 2(prepares tire chrysanthemum hydrosol by method of the present invention)
A kind of tire chrysanthemum hydrosol, preparation method preparation in accordance with the following steps:
(2) pretreatment: the tire chrysanthemum flower plucked tire chrysanthemum planting base is spread out in indoor and dried in the shade;
(2) feed intake, infiltrate: tire chrysanthemum 50kg step 1 dried in the shade drops in distillating still, add 150kg deionized water to soak, soak time is 1 hour, be interrupted in immersion process and carry out low rate mixing, opened every 15 minutes and once stir, mixing speed 10-15 rev/min, each mixing time is 1-2 minute;
(3) ultrasonic Treatment: first mixing speed is controlled, at 10-15 rev/min, then to open heater, heating material in distillating still is warming up to 85 DEG C; Frequency is adopted to be the ultrasonic Treatment 15 minutes of 20kHZ;
(4) distill: after ultrasonic Treatment, material in distillating still is heated to 100 DEG C, open the condenser of distillating still, and the cooling water that circulates within the condenser, start to collect distillate, what in still-process, adjust distillate distillates speed, makes the gathering speed of distillate control at 40kg/ hour, terminates distillation after 4 hours;
(5) clarify: the distillate collected is left standstill 12 hours, extracts the supernatant, turbid for bottom liquid 1000 order filter clothes are filtered simultaneously, filtrate and the supernatant are merged;
(6) filter at low temperature: the distillate of clarification step 5 obtained preserves 24h under 2-3 DEG C of cryogenic conditions, then use the filter plant pressure filtration of aperture 1-2 micron.
(7) anticorrosion: to filter to step 6 in the filtrate of gained and add antiseptic, its addition of antiseptic is 0.5% of filtrate quality, and antiseptic is 1,2-hexanediol and 1, the 2-ethohexadiol of mass ratio 1:1.
(8) filling and package: according to packing specification in dust proof workshop fill, treats that end product quality after the assay was approved, and product good for fill is carried out labeling, stamp, vanning, packing, warehouse-in.
The tire chrysanthemum hydrosol that embodiment 2 obtains is through quality testing, and its microbiological indicator meets all standard above shown in table 1; Physical and chemical index assay and sense organ meet the requirements of table 2.Obtained tire chrysanthemum hydrosol fragrance is pure, and have the tire chrysanthemum fragrance of fragrance, steady quality, places and also do not separate out precipitate in 3 years, and appearance transparent is clarified.
Comparative example 1(prepares tire chrysanthemum hydrosol by traditional hydrosol preparation method)
The tire chrysanthemum hydrosol hydrosol preparation method preparation traditionally of comparative example 1, concrete steps are:
(1) pretreatment: tire chrysanthemum flower is spread out in indoor and dries in the shade;
(2) feed intake, infiltrate: tire chrysanthemum 100kg step 1 dried in the shade drops in distillating still, adding containing 1%-5%(weight) the deionized water 300kg of Sal soaks, be interrupted in immersion process and carry out low rate mixing, opened every 10-20 minute and once stir, mixing speed 10-15 rev/min, mixing time 1-2 minute;
(3) distill: heating material in distillating still is warmed up to 100 DEG C, opens the condenser of distillating still, and the cooling water that circulates within the condenser, imported in oil water separator by the distillate collected, the temperature of oil water separator controls at 25-35 DEG C;
(4) hydrosol is collected: after oil water separator is separated, distillate is divided into water layer and oil reservoir, and by water layer distillate resurgent in distillating still, the resurgent persistent period is 3 hours, closes resurgent valve afterwards, opens collection valve, start to collect water layer.
(5) quintessence oil is collected: distillate, after oil water separator is separated, is treated the abundant layering of profit, opened oil water separator, collects oil reservoir and namely obtains tire chrysanthemum quintessence oil;
(6) clarify: by step 4 collect water layer leave standstill 12-24 hour, extract the supernatant, turbid for bottom liquid is filtered simultaneously, filtrate and the supernatant is merged, obtain tire chrysanthemum hydrosol product.
After testing, its Comparative result is as shown in table 3 below for the tire chrysanthemum hydrosol product of embodiment 1 ~ 2 and comparative example 1:
Table 3
Effect detection:
Detection results on probation is carried out to tire chrysanthemum hydrosol prepared by embodiment 1, simultaneously present inventor with the tire chrysanthemum hydrosol of comparative example 1 for contrast.
Detected object: the tire chrysanthemum hydrosol of embodiment 1 and comparative example 1 is tried out 30 days continuously through 100 personnel (face has skin sore small pox) respectively.Using method: with the cotton pads full face of wiping gently after clean, use 2 every day, use 4 weeks.Paper examines three aspect: humidity of skin, skin smoothness and acne removing effect.
Testing result sees the following form 4.
Table 4
Also carry out effect detection to the tire chrysanthemum hydrosol of embodiment 2, testing result finds that the trial effect of embodiment 2 is similar with embodiment 1 result, does not repeat them here.Facts have proved, the tire chrysanthemum hydrosol that the present invention obtains has better replenishing water and preserving moisture, heat clearing away toxin expelling, skin maintenance effect, and whiteness of skin can be made tender, is rich in gloss elasticity, skin sore small pox reduces.After on probation, tire chrysanthemum hydrosol prepared by the present invention does not find chafe and allergic phenomena.
Claims (8)
1. a preparation method for tire chrysanthemum hydrosol, is characterized in that, comprises the steps:
(1) pretreatment: tire chrysanthemum flower is spread out in indoor and dries in the shade;
(2) feed intake, infiltrate: tire chrysanthemum 50 ~ 100kg step (1) dried in the shade drops in distillating still, adds 150 ~ 300kg deionized water and soaks, be interrupted in immersion process and carry out low rate mixing;
(3) ultrasonic Treatment: mixing speed controlled at 10-15 rev/min, opens the heater of distillating still, and heating material in distillating still is warming up to 85-90 DEG C, then adopts frequency to be the ultrasonic Treatment 10-15 minute of 20KHz;
(4) distill: after ultrasonic Treatment, heating material in distillating still is warmed up to 100 DEG C, opens the condenser of distillating still, and the cooling water that circulates within the condenser, start to collect distillate;
(5) clarify: the distillate of collection is left standstill 12-24 hour, extract the supernatant, turbid for bottom liquid is filtered simultaneously, filtrate and the supernatant are merged;
(6) filter at low temperature: the product that step (5) obtains is preserved 24-48h under 2-3 DEG C of cryogenic conditions, then use the filter plant pressure filtration of aperture 1-2 micron.
2. the preparation method of tire chrysanthemum hydrosol according to claim 1, it is characterized in that, described preparation method also has step (7), step (7) is: filter to step (6) in the filtrate of gained and add antiseptic, its addition of described antiseptic is 0.3 ~ 0.5% of filtrate quality.
3. the preparation method of tire chrysanthemum hydrosol according to claim 2, is characterized in that, described antiseptic is 1, the 2-hexanediol and 1,2-ethohexadiol that mix according to the mass ratio of 1:1 ~ 3.
4. the preparation method of tire chrysanthemum hydrosol according to claim 1, it is characterized in that, interruption described in step (2) carry out low rate mixing refer in immersion process every 10-20 minute open once stir, mixing speed 10-15 rev/min, each mixing time is 1-2 minute.
5. the preparation method of tire chrysanthemum hydrosol according to claim 1, is characterized in that, in step (5), the turbid liquid of bottom adopts 400 ~ 1000 object filter clothes to filter.
6. the preparation method of tire chrysanthemum hydrosol according to claim 1, is characterized in that, the gathering speed of distillate controls at 40 ~ 50kg/ hour in (4) by step.
7. the preparation method of tire chrysanthemum hydrosol according to claim 1, is characterized in that, the persistent period that step (4) carries out distilling is 3 ~ 4 hours.
8. the tire chrysanthemum hydrosol obtained by the preparation method described in any one of claim 1 ~ 7.
Priority Applications (1)
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| CN103735459B (en) * | 2013-12-27 | 2015-09-02 | 宗欣生态科技(上海)有限公司 | There is plant extract of skin and complexion improving effect and uses thereof |
| CN104257533A (en) * | 2014-08-28 | 2015-01-07 | 李伟安 | Novel preparation method of plant washing liquid |
| CN104367510A (en) * | 2014-11-13 | 2015-02-25 | 青岛厚科信息工程有限公司 | Natural extract body wash and preparation method thereof |
| CN104940054A (en) * | 2015-05-30 | 2015-09-30 | 防城港市防城区那梭香料厂 | Preparation method of pure natural lemon lemongrass hydrolat |
| CN104856905A (en) * | 2015-05-30 | 2015-08-26 | 防城港市防城区那梭香料厂 | Hydrolat containing cymbopogon citratus |
| CN105055239A (en) * | 2015-08-13 | 2015-11-18 | 刘汉科 | Peppermint hydrolat lotion and preparation method thereof |
| CN105055238A (en) * | 2015-08-13 | 2015-11-18 | 刘汉科 | Neroli hydrolat lotion and preparation method thereof |
| CN106074290A (en) * | 2016-07-25 | 2016-11-09 | 谭志华 | A kind of looks improving and the skin nourishing facial mask powder |
| CN106511142A (en) * | 2017-01-18 | 2017-03-22 | 广西南宁博智生物科技有限公司 | Centella asiatica floral water and preparation method and application thereof |
| CN107011993B (en) * | 2017-03-30 | 2020-10-16 | 韩后化妆品股份有限公司 | Compound essential oil and preparation method thereof |
| CN107157861B (en) * | 2017-07-17 | 2020-08-07 | 重庆市日用化学工业研究所 | Chrysanthemum hydrolat and beauty fluid prepared from same |
| CN108323547A (en) * | 2018-04-19 | 2018-07-27 | 长春职业技术学院 | Flower class essential oil health-care bread |
| CN108743457A (en) * | 2018-06-19 | 2018-11-06 | 广州叁合人生物科技有限公司 | A kind of compound essential oil with effect of weight reducing |
| CN110894438A (en) * | 2018-09-12 | 2020-03-20 | 苏州市元使生物科技有限公司 | Biluochun tea pure dew refining process |
| CN111728109A (en) * | 2020-06-19 | 2020-10-02 | 红河大自然水业有限责任公司 | Preparation method of edible flower hydrolat |
| CN113768015A (en) * | 2021-09-24 | 2021-12-10 | 尹帅 | Preparation method of keemun chrysanthemum water |
| CN114028280A (en) * | 2021-11-19 | 2022-02-11 | 陕西蒲城兴农生物科技开发有限公司 | Taxus chinensis hydrolat and preparation method thereof |
| CN114989890A (en) * | 2022-05-25 | 2022-09-02 | 湖南诺泽生物科技有限公司 | Cumin essential oil and preparation method and application thereof |
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| 德国甘菊蒸馏水有机成分分析研究;张运晖 等;《上海交通大学学报（农业科学版）》;20101231;第28卷(第6期);第546-551页 * |
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