Summary of the invention
The object of the invention is to solve above-mentioned technical problem, a kind of tomato leaf method for preparing extractive of simple, efficient, environmental protection is provided, and the tomato leaf extract of preparing is applied in cosmetics, play the crease-resistant effect of beauty treatment.
Object of the present invention is achieved through the following technical solutions:
A preparation method for tomato leaf extract, comprises following steps:
Step 1, pulverizing: dry tomato leaf is crushed to 100 orders;
Step 2, slightly extraction: the aqueous solution that preparation contains sodium sulfite, then add ethanol, obtain solution.In the tomato leaf crushed material of step 1, add this solution, crushed material than for 1:10 ~ 1:20, extracts 4-6 hour with solution quality at 60-90 ℃ of temperature, repeats to extract three times;
Step 3, filtration drying: the crude extract of step 2 is cooled to 20-30 ℃, with 1000-2000 order filter cloth filtering insoluble matter, is evaporated to 1/5 to 1/10 of extracting liquid volume in step 2, then carry out vacuum drying and obtain dry;
Step 4, dissolving are refined: at the dry that step 3 is obtained, adding solvent, the mass volume ratio of dry and solvent is 1:5, stand at low temperature 1-2 days, in centrifuge with the centrifugal 30min of rotating speed 5000rpm, collect supernatant, obtain refining tomato leaf extract.
Therein in some embodiment, the described ethanol volumetric concentration of slightly carrying in the solution that step makes is 30-50%, and described dissolving purification step stand at low temperature temperature is-10 ℃ ~ 0 ℃.
In some embodiment, the mass fraction of described sodium sulfite in aqueous solution is 0.1-0.5% therein.
Sodium sulfite of the present invention, is the antioxidant that a kind of permission is directly added in cosmetics, and sodium sulfite plays the at high temperature oxidized effect such as the readily oxidizable substance that prevents vitamin C, folic acid in the manufacture of tomato leaf extract.Its addition selects the reason of 0.1%-0.5% to be in the present invention, the present inventor finds when the addition of sodium sulfite is lower than 0.1% time in experiment, the antioxidant effect being risen is not obvious, and easily in the alcoholic solution that is 30-50% containing volumetric concentration, separates out higher than 0.5% time when its addition.
In the preferred embodiment of the present invention, described solvent is one or more replacements in ethanol, propylene glycol, glycerol, PEG-4000, dipropylene glycol, 1,3 butylene glycol etc.Preferably, described solvent is 1,3 butylene glycol.
The present invention also provides according to the prepared tomato leaf extract of above-mentioned preparation method, in the middle of described tomato leaf extract, and general flavone content >=8Wt%, Vitamin C content >=0.3Wt%.
The present invention also provides according to above-mentioned tomato leaf extract in the application of preparing in cosmetics.
Therein in some embodiment, described tomato leaf extract is in the application of preparing in cosmetics, comprise substrate and tomato leaf extract, described substrate is vegetable and animals oils, mineral oil, wax, higher alcohol, fatty alcohol, silicone oil, surfactant, phospholipid, alcohols, polyalcohols, water-soluble polymer, oil-soluble polymers, mineral or deionized water, and the dosage form of described cosmetics is water preparation, cream, washing liquid or emulsion.
The present invention with respect to advantage and the beneficial effect of prior art is:
1, the present invention takes full advantage of natural plants, has expanded the Application and Development field of tomato leaf;
2, the present invention, preparing in the process of tomato leaf extract, only passes through filtration, dry, centrifugal, standing several processes, and whole extraction process is simple and easy to operate, and production cost is low; But the content of the active component in extract still reaches higher level;
3, the present invention, in leaching process, only uses water, ethanol, three kinds of solvents of 1,3 butylene glycol, does not introduce other extraction organic solvent, by cryogenic freezing technology, promotes sedimentary extraction to separate out, then centrifugalize, is a kind of preparation technology of environmental protection.
the specific embodiment
In following embodiment, polyacrylamide/C13-14 isoparaffin/laureth-7 are commercially available prod, and commodity are called SEPIGEL 305, originate from France match BIC Corp.
Below in conjunction with preferred specific embodiment, the invention will be further described.
Embodiment 1
A preparation method for tomato leaf extract, comprises following steps:
Step 1, pulverizing: dry tomato leaf is crushed to 100 orders;
Step 2, slightly extract: the preparation mass fraction aqueous solution of sodium bisulfite that is 0.1%, then to add ethanol to ethanol volumetric concentration be 30%, obtains solution.In the tomato leaf crushed material of step 1, add this solution, crushed material than for 1:10 ~ 1:20, extracts 4-6 hour with solution quality at 60-90 ℃ of temperature, repeats to extract three times;
Step 3, filtration drying: the crude extract of step 2 is cooled to 20-30 ℃, with 1000-2000 order filter cloth filtering insoluble matter, is evaporated to 1/5 to 1/10 of extracting liquid volume in step 2, then carry out vacuum drying and obtain dry;
Step 4, dissolving are refined: at the dry that step 3 is obtained, adding 1,3 butylene glycol, dry and 1, the mass volume ratio of 3-butanediol is 1:5 ,-10 ℃ static 2 days, in centrifuge with the centrifugal 30min of rotating speed 5000rpm, collect supernatant, obtain refining tomato leaf extract.
Embodiment 2
A preparation method for tomato leaf extract, comprises following steps:
Step 1, pulverizing: dry tomato leaf is crushed to 100 orders;
Step 2, slightly extract: preparation mass fraction is 0. 3% aqueous solution of sodium bisulfite, then to add ethanol to ethanol volumetric concentration be 50%, obtain solution.In the tomato leaf crushed material of step 1, add this solution, crushed material than for 1:10 ~ 1:20, extracts 4-6 hour with solution quality at 60-90 ℃ of temperature, repeats to extract three times;
Step 3, filtration drying: the crude extract of step 2 is cooled to 20-30 ℃, with 1000-2000 order filter cloth filtering insoluble matter, is evaporated to 1/5 to 1/10 of extracting liquid volume in step 2, then carry out vacuum drying and obtain dry;
Step 4, dissolving are refined: at the dry that step 3 is obtained, adding 1,3 butylene glycol, dry and 1, the mass volume ratio of 3-butanediol is 1:5 ,-5 ℃ static 1 day, in centrifuge with the centrifugal 30min of rotating speed 5000rpm, collect supernatant, obtain refining tomato leaf extract.
Embodiment 3
A preparation method for tomato leaf extract, comprises following steps:
Step 1, pulverizing: dry tomato leaf is crushed to 100 orders;
Step 2, slightly extract: the preparation mass fraction aqueous solution of sodium bisulfite that is 0.5%, then to add ethanol to ethanol volumetric concentration be 40%, obtains solution.In the tomato leaf crushed material of step 1, add this solution, crushed material than for 1:10 ~ 1:20, extracts 4-6 hour with solution quality at 60-90 ℃ of temperature, repeats to extract three times;
Step 3, filtration drying: the crude extract of step 2 is cooled to 20-30 ℃, with 1000-2000 order filter cloth filtering insoluble matter, is evaporated to 1/5 to 1/10 of extracting liquid volume in step 2, then carry out vacuum drying and obtain dry;
Step 4, dissolving are refined: at the dry that step 3 is obtained, adding 1,3 butylene glycol, dry and 1, the mass volume ratio of 3-butanediol is 1:5,0 ℃ static 2 days, in centrifuge with the centrifugal 30min of rotating speed 5000rpm, collect supernatant, obtain refining tomato leaf extract.
The performance test of embodiment 4 tomato leaf extracts
One, the stability test of tomato leaf extract
Get the transparent test bottle that 6 capacity are 100g, fill the prepared tomato leaf extract of the present embodiment 1, in room temperature (20 ± 1) ℃, heat-resisting (45 ± 1) ℃, cold-resistant (5 ± 1) ℃, do stability test.Result is as shown in table 1-table 4.
Table 1: the first peripheral stability test result.
Table 2: second week stability test result.
Table 3: the 3rd peripheral stability test result.
Table 4: 4th week stability test result.
From table 1-table 4, tomato leaf extract energy long-term stability prepared by the present invention is deposited.
Two, the human body patch of tomato leaf extract experiment
The human body skin patch Experimental Standardization of organizing 30 volunteers to record according to < < cosmetics health standard > > (2007 editions), the prepared tomato leaf extract of the test embodiment of the present invention 1, result is as shown in table 5.
Table 5: patch test
Tested object | Content measurement | Test result | Judgement |
30 volunteers | The experiment of skin enclosed type patch | 30 routine experimenters are negative reaction | Judge the Potential feasibility that tested material has no adverse reaction to human body skin |
Three, the vitamin C of tomato leaf extract and general flavone content test
3.1 test purpose
3.1.1 record vitamin C and general flavone content in the prepared tomato leaf extract of the embodiment of the present invention;
3.1.2 investigate tomato leaf method for preparing extractive and slightly propose the impact of ethanol volumetric concentration on vitamin C in extract and general flavone content in step solution.
3.2 method of testing
Comparative example 1
A preparation method for tomato leaf extract, comprises following steps:
Step 1, pulverizing: dry tomato leaf is crushed to 100 orders;
Step 2, slightly extract: the preparation mass fraction aqueous solution of sodium bisulfite that is 0.1%, then to add ethanol to ethanol volumetric concentration be 20%, obtains solution.In the tomato leaf crushed material of step 1, add this solution, crushed material than for 1:10 ~ 1:20, extracts 4-6 hour with solution quality at 60-90 ℃ of temperature, repeats to extract three times;
Step 3, filtration drying: the crude extract of step 2 is cooled to 20-30 ℃, with 1000-2000 order filter cloth filtering insoluble matter, is evaporated to 1/5 to 1/10 of extracting liquid volume in step 2, then carry out vacuum drying and obtain dry;
Step 4, dissolving are refined: at the dry that step 3 is obtained, adding 1,3 butylene glycol, dry and 1, the mass volume ratio of 3-butanediol is 1:5 ,-10 ℃ static 2 days, in centrifuge with the centrifugal 30min of rotating speed 5000rpm, collect supernatant, obtain refining tomato leaf extract.
Comparative example 2
A preparation method for tomato leaf extract, comprises following steps:
Step 1, pulverizing: dry tomato leaf is crushed to 100 orders;
Step 2, slightly extract: the preparation mass fraction aqueous solution of sodium bisulfite that is 0.1%, then to add ethanol to ethanol volumetric concentration be 60%, obtains solution.In the tomato leaf crushed material of step 1, add this solution, crushed material than for 1:10 ~ 1:20, extracts 4-6 hour with solution quality at 60-90 ℃ of temperature, repeats to extract three times;
Step 3, filtration drying: the crude extract of step 2 is cooled to 20-30 ℃, with 1000-2000 order filter cloth filtering insoluble matter, is evaporated to 1/5 to 1/10 of extracting liquid volume in step 2, then carry out vacuum drying and obtain dry;
Step 4, dissolving are refined: at the dry that step 3 is obtained, adding 1,3 butylene glycol, dry and 1, the mass volume ratio of 3-butanediol is 1:5 ,-10 ℃ static 2 days, in centrifuge with the centrifugal 30min of rotating speed 5000rpm, collect supernatant, obtain refining tomato leaf extract.
Get the each 100g of the prepared tomato leaf extract of embodiment 1-3 and comparative example 1-2, mensuration Vitamin C content (referring to: the interim < < fruit of [spectrographic laboratory] the 23rd volume the 4th, in vegetable, mensuration-uv-spectrophotometric rapid assay methods of Vitamin C content is inquired into > >) and general flavone content (referring to: the wild Dendrocalamus giganteus Munro Folium Bambosae flavone content of < < that [western forest-science] the 42nd volume the 2nd is interim and Antioxidative Activity Determination experiment > > thereof), test result is as following table 6:
Table 6: working substance content
? | Embodiment 1 | Embodiment 2 | Embodiment 3 | Comparative example 1 | Comparative example 1 |
Total flavones (mg/100g) | 8210.1 | 8105.0 | 8127.5 | 2531.4 | 4230.2 |
Vitamin c (mg/100g) | 342.1 | 325.4 | 305.2 | 114.7 | 156.2 |
As can be seen from Table 6, in the tomato leaf extract that the present embodiment 1-3 makes, vitamin C average content is 324.2mg/100g, and total flavones average content is 8147.5mg/100g, can approximate representation be in this extract, general flavone content >=8Wt%, Vitamin C content >=0.3Wt%.In addition, the prepared Vitamin C content of comparative example 1-2 and general flavone content be all lower than embodiment 1-3, illustrates in the thick extraction step solution of tomato leaf method for preparing extractive that ethanol volumetric concentration is controlled at 30%-50% more excellent.
Four, the antioxidant activity of tomato leaf extract test
4.1 test purpose
4.1.1 measure the antioxidant activity of tomato leaf extract prepared by the present invention;
4.1.2 the impact of the mass percent of investigating sodium sulfite in the thick extraction step solution of tomato leaf method for preparing extractive on extract antioxidant activity.
4.2 method of testing
Comparative example 3:
A preparation method for tomato leaf extract, comprises following steps:
Step 1, pulverizing: dry tomato leaf is crushed to 100 orders;
Step 2, slightly extract: the preparation mass fraction aqueous solution of sodium bisulfite that is 0.05%, then to add ethanol to ethanol volumetric concentration be 30%, obtains solution.In the tomato leaf crushed material of step 1, add this solution, crushed material than for 1:10 ~ 1:20, extracts 4-6 hour with solution quality at 60-90 ℃ of temperature, repeats to extract three times;
Step 3, filtration drying: the crude extract of step 2 is cooled to 20-30 ℃, with 1000-2000 order filter cloth filtering insoluble matter, is evaporated to 1/5 to 1/10 of extracting liquid volume in step 2, then carry out vacuum drying and obtain dry;
Step 4, dissolving are refined: at the dry that step 3 is obtained, adding 1,3 butylene glycol, dry and 1, the mass volume ratio of 3-butanediol is 1:5 ,-10 ℃ static 2 days, in centrifuge with the centrifugal 30min of rotating speed 5000rpm, collect supernatant, obtain refining tomato leaf extract.
Get the each 100g of the prepared tomato leaf extract of embodiment 1 and comparative example 3, measure antioxidant activity (referring to Wang Qi, Tian Diying, Yang Ronghua by DPPH method, the comparison of fruit and vegerable Antioxidative Activity Determination method, [food and fermentation industries] 5 phases in 2008), the antioxidant activity that records the prepared tomato leaf extract of embodiment 1 is 95.73%, and the antioxidant activity of the prepared tomato leaf extract of comparative example 3 is 60.21%.Illustrate that the prepared tomato leaf extract of the embodiment of the present invention has good antioxidant activity, it is more excellent that the mass percent that sodium sulfite in the thick extraction step solution of tomato leaf method for preparing extractive is also described is controlled at 0.1-0.5%.
Five, be added with the crease-resistant effect of beauty treatment of the cosmetics of tomato leaf extract.
Tomato leaf extract is applied in the cosmetics of each dosage form, the substrate of these cosmetics be vegetable and animals oils, mineral oil, wax, higher alcohol, fatty alcohol, silicone oil, surfactant, phospholipid, alcohols, polyalcohols, water-soluble polymer, oil-soluble polymers class, mineral or deionization who, the dosage form of cosmetics is water preparation, cream, washing liquid or emulsion.
Below illustrate dosage form example of the present invention.
[dosage form example 1] cosmetic water
The component that toner/smoothing toner comprises following mass percent: glycerol 5%, propylene glycol 5%, 1,3 butylene glycol 5%, allantoin 1%, hyaluronate sodium 0.05%, tomato leaf extract 5%, cellulose gum 0.01%, antiseptic 0.2%, water surplus.
This cosmetic water can be prepared by following technique: glycerol, propylene glycol, 1,3 butylene glycol, allantoin, hyaluronate sodium, cellulose gum, water are joined in agitated kettle, be heated to 85 ℃; Stirring is cooled to 30-40 ℃ and adds antiseptic, tomato leaf extract.
[dosage form example 2] essence cream
The component that essence cream comprises following mass percent: cetearyl alcohol 2%, caprylic/capric triglyceride 5%, squalane 3%, polydimethylsiloxane 2%, ring five polydimethylsiloxane 5%, glycerol 5%, 1,3 butylene glycol 3%, allantoin 0.2%, tomato leaf extract 5%, HANSHENGJIAO 0.3%, polyacrylamide and C13-14 isoparaffin and cinnamic alcohol ether-7 0.8%, antiseptic 0.3%, water surplus.
This essence cream can be prepared by following technique: cetearyl alcohol, caprylic/capric triglyceride, squalane, polydimethylsiloxane, ring five polydimethylsiloxane are added in oil phase pot as A, are heated to 80 ℃; Glycerol, 1,3 butylene glycol, allantoin, HANSHENGJIAO, water are added in emulsifying pot as B, are heated to 80 ℃; A is added to B phase homogenizing 2-3 minute; Add polyacrylamide and C13-14 isoparaffin and cinnamic alcohol ether-7 homogenizing 2-3 minute; Stirring is cooled to 30-40 ℃ and adds tomato leaf extract, antiseptic.
The prepared essence cream of dosage form example 2 is carried out to the evaluation of atraumatic human body, as a control group with a commercially available cream frost that lays claim to the crease-resistant effect of good beauty treatment simultaneously.
Tested object: each experimental group is 20 women (35-50 year); Test zone: crows-feet region; Use: every day twice, continue to use 4 weeks; Test event: the soft degree of skin, wrinkle depth (crows-feet region).Result on trial refers to table 7.
Table 7: atraumatic human body evaluation test result
As can be seen from Table 7, the prepared essence cream of the present invention has shown good beauty treatment anti-wrinkle effect compared with matched group commercially available prod.
By above physicochemical property detection, human body patch test and atraumatic human body, evaluate, prove that tomato leaf extract is a kind of steady quality, index and definite ingredients, there is the vegetable raw material of the crease-resistant effect of beauty treatment, safe and non-stimulating, can be used as independent or composite other function raw material of function raw material and use in the cosmetics of any dosage form.
The above embodiment has only expressed several embodiment of the present invention, and it describes comparatively concrete and detailed, but can not therefore be interpreted as the restriction to the scope of the claims of the present invention.It should be pointed out that for the person of ordinary skill of the art, without departing from the inventive concept of the premise, can also make some distortion and improvement, these all belong to protection scope of the present invention.Therefore, the protection domain of patent of the present invention should be as the criterion with claims.