A kind of Exocarpium Citri Grandises leaf naringin and Radix seu Folium Tosicodendri Delavayi glucoside sunscreen cream and preparation method thereof
Technical field
The present invention relates to cosmetic field, specifically a kind of Exocarpium Citri Grandises leaf naringin and Radix seu Folium Tosicodendri Delavayi glucoside sunscreen cream and its preparation
Method.
Background technology
Ultraviolet can be divided into shortwave(200~275nm), medium wave(275~320nm)And long wave(320~400nm).Shortwave
Ultraviolet energy is the strongest, and short irradiation gets final product skin ambustion, and long-term irradiation also can produce skin carcinoma.But because can be by hemisphere
25 kilometers of ozone layer absorbs, and skin will not be damaged.Ultraviolet B radiation is referred to as " B area ultraviolet(UVB)", to people
Body has erythema effect, can promote the formation of internal mineral metabolism and vitamin D, but long-term or excessive exposure can make skin shine
Black, and cause red and swollen decortication, it is sun-proof emphasis wave band.Long wave ultraviolet is referred to as " A area ultraviolet(UVA)", there is very strong wearing
Thoroughly power, UVA can go directly the skin corium of skin, and the energy reaching skin is up to more than the 98% of ultraviolet gross energy, destroys bullet
Property fiber and collagen fabric, cause unmanageable skin injury, become Pigmented immediate cause, such as form passeris montani saturati
Speckle, senile plaque etc..So long wave ultraviolet encourages the injury to skin for the medium wave, promote skin aging.Therefore, develop efficient, peace
Entirely, the wide ultraviolet product of natural anti-wave-length coverage easy to use is just subject to people's attention.
Abundant flavonoid naringin and Radix seu Folium Tosicodendri Delavayi glucoside is contained in Exocarpium Citri Grandises leaf(Total amount accounts for leaf dry 6~13.6%), leaf
Age is less, and the total content of flavonoid is higher, and the ratio of Radix seu Folium Tosicodendri Delavayi glucoside is bigger, in the tender leaf just extracted out the content of Radix seu Folium Tosicodendri Delavayi glucoside also than
The height of naringin.Naringin has two absworption peaks in ultraviolet ray range, and, in 283 nm, secondary peak is in 330 nm, Rhus succedanea for main peak
Glycosides also has two absworption peaks, main peak in 340 nm, secondary peak in 261 nm, therefore, both the absorption of ultraviolet is played collaborative and
Complementary action, two kinds of flavonoid are blended in ultraviolet ray range(200~400nm)All there is strong absorption.Meanwhile, naringin and open country
Toxicodendron verniciflnum (Stokes) F. A. Barkley (Rhus verniciflua Stokes) glycosides has allaying tiredness, protection blood vessel, expansion capillary tube, dredging microcirculation, the work(of fat anti-oxidation, skin protection and defying age
Energy.
Exocarpium Citri Grandises are the rare Chinese medicines of preventing phlegm from forming and stopping coughing, and Exocarpium Citri Grandises leaf and fruit are all containing volatile oil, flavonoid and polysaccharide etc.
Active component.The 2~6.8% of dry is accounted for containing Exocarpium Citri Grandises characteristic flavone Radix seu Folium Tosicodendri Delavayi glucoside, than the plant material in other sources in leaf
The content of material pummelo peel fruit and leaf of Turpinia pomifera (Roxb) D O. is much higher.Exocarpium Citri Grandises nourish and grow speed soon, take out slightly 3~5 times year, branch and leaf yield
Huge, current Guangdong Huazhou City and about 200000 mu of surrounding area Exocarpium Citri Grandises cultivated area, and with the annual speed increasing by 10000 mu
Degree expands planting scale, and therefore, the resource provisioning of Exocarpium Citri Grandises leaf flavonoid is sufficient.
The flavonoid being extracted using 95% food-grade ethanol, is removed chromophyll with isopyknic petroleum ether extraction, washes with water
Water-solubility impurity, crude flavonoid powder total amount accounts for more than 98% that leaf dry 7~14%, wherein naringin and Radix seu Folium Tosicodendri Delavayi glucoside account for total flavones.
There is not been reported for the research of the Flavonoid substances naringin and Radix seu Folium Tosicodendri Delavayi glucoside defense function aspect to ultraviolet.
Content of the invention
It is an object of the invention to provide a kind of Exocarpium Citri Grandises leaf naringin and Radix seu Folium Tosicodendri Delavayi glucoside sunscreen cream and preparation method thereof, with
Solve the problems, such as to propose in above-mentioned background technology.
For achieving the above object, the present invention provides following technical scheme:
A kind of Exocarpium Citri Grandises leaf naringin and Radix seu Folium Tosicodendri Delavayi glucoside sunscreen cream, are prepared from by the raw material of following weight fraction:Naringin and
Radix seu Folium Tosicodendri Delavayi glucoside mixture 0.2~2.0%, Cera Flava 9~18%, ammonia ketone 0.1~1.0%, glycerol 2~20%, preservative 0.1~
1.0%, balance of deionized water.
As the further scheme of the present invention:The preparation process of described naringin and Radix seu Folium Tosicodendri Delavayi glucoside mixture is:
(1)Pluck Exocarpium Citri Grandises tender leaf to clean, the sun dries or puts in baking oven 50~60 DEG C dries to constant weight, pulverizes 40~50 mesh
Sieve, obtains leaf powder;
(2)Leaf powder is loaded in glass chromatography column, 95% food-grade ethanol makees extracting solution, in post, soak 50~70min, eluting
Flow velocity 95~105 mL/h, collects eluent;
(3)The eluent of collection is carried out rotary evaporation in vacuo and is concentrated into paste;
(4)The concentrated solution of paste is transferred to separatory funnel, addition equivalent volumes petroleum ether extraction 3~4 times, removes upper liquid,
Obtain lower floor's extraction mixture;
(5)Lower floor's extraction mixture of gained is carried out rotary evaporation in vacuo be concentrated to dryness, washed with cold water 3~4 times, obtain Fructus Citri grandiss
Skin glycosides and Radix seu Folium Tosicodendri Delavayi glucoside mixture.
As the present invention further scheme:Described preservative is potassium sorbate.
A kind of described Exocarpium Citri Grandises leaf naringin and the preparation method of Radix seu Folium Tosicodendri Delavayi glucoside sunscreen cream, concrete preparation process is as follows:
(1)Cera Flava is heated to 65~90 DEG C, stirring and dissolving, to uniform, as oil phase A, is incubated standby;
(2)Glycerol is added mix homogeneously in deionized water, as B phase, standby;
(3)Naringin and Radix seu Folium Tosicodendri Delavayi glucoside mixture are dissolved in B phase, and are heated to 65~90 DEG C, be slowly stirred, mix homogeneously,
As C phase;
(4)The C phase of gained is slowly added in A phase, and adds ammonia ketone, carry out high-speed stirred 3~5min simultaneously, mixing is all
Even;
(5)By step(4)The mixture of gained is cooled to 75~80 DEG C, is slowly stirred, and carries out froth breaking;
(6)After the completion of froth breaking, be cooled to 45 DEG C, add preservative, continue to be slowly stirred, to be cooled be cooled to room temperature, stop stirring
Mix;
(7)By step(6)The mixture obtaining is ground as pasty mixture, and fineness of the particles is less than 5 μm;
(8)By the pasty mixture after grinding, it is paste semi-finished product that input homogenizer carries out high speed strong stirring;
(9)By step(8)The paste semi-finished product of gained carry out vacuum degassing process process, fill, you can.
Compared with prior art, the invention has the beneficial effects as follows:
Present invention column chromatography extracts naringin and Radix seu Folium Tosicodendri Delavayi glucoside in Exocarpium Citri Grandises leaf, and post processing extraction solvent consumption is few, and extraction ratio is high.
Naringin and Radix seu Folium Tosicodendri Delavayi glucoside mixture to ultraviolet absorption ability in different wave length complimentary to one another be superimposed, therefore, in ultraviolet
Absorb strong and uniform in the range of line, be good anti-ultraviolet activating agent.Because it has sun-proof, free radical resisting reparation effect
Really, apply on sunscreen cream as a kind of sunscreen, have that zest is low, sun-proof result is good, free radical resisting, lighter color, not shadow
Ring the feature of product colour, and the preparation process is simple of this sunscreen and corresponding sunscreen cream is feasible.
Brief description
Fig. 1 is the uv absorption spectra of naringin and Radix seu Folium Tosicodendri Delavayi glucoside.
Fig. 2 is the ultra-violet absorption spectrum compares figure of product of the present invention and the two brand sunscreen cream in market.
Specific embodiment
Below in conjunction with the accompanying drawing in the embodiment of the present invention, the technical scheme in the embodiment of the present invention is carried out clear, complete
Site preparation description is it is clear that described embodiment is only a part of embodiment of the present invention, rather than whole embodiments.It is based on
Embodiment in the present invention, it is every other that those of ordinary skill in the art are obtained under the premise of not making creative work
Embodiment, broadly falls into the scope of protection of the invention.
Embodiment 1
Exocarpium Citri Grandises leaf naringin and Radix seu Folium Tosicodendri Delavayi glucoside sunscreen cream, are prepared from by the raw material of following weight fraction:Naringin and wild paint
Tree glycosides mixture 1.0%, Cera Flava 18%, ammonia ketone 0.7%, glycerol 15%, potassium sorbate 0.6%, balance of deionized water.
The preparation process of naringin and Radix seu Folium Tosicodendri Delavayi glucoside mixture is:
(1)Pluck Exocarpium Citri Grandises tender leaf to clean, the sun dries or puts in baking oven 58 DEG C dries to constant weight, pulverized 40 mesh sieves, and obtained leaf
Powder;
(2)Leaf powder is loaded in glass chromatography column, 95% food-grade ethanol makees extracting solution, in post, soak 50min, eluting liquor stream
Fast 105mL/h, collects eluent;
(3)The eluent of collection is carried out rotary evaporation in vacuo and is concentrated into paste;
(4)The concentrated solution of paste is transferred to separatory funnel, addition equivalent volumes petroleum ether extraction 3 times, removes upper liquid, obtain
Lower floor's extraction mixture;
(5)Lower floor's extraction mixture of gained is carried out rotary evaporation in vacuo be concentrated to dryness, washed with cold water 4 times, obtain Pericarpium Citri grandiss
Glycosides and Radix seu Folium Tosicodendri Delavayi glucoside mixture.
The preparation process of above-mentioned sunscreen cream is as follows:
(1)Solid Cera Flava will be taken to be heated to 70 DEG C, stirring and dissolving, as the insulation of A phase, standby;
(2)Glycerol is added in deionized water, as B phase, standby;
(3)Naringin and Radix seu Folium Tosicodendri Delavayi glucoside mixture are dissolved in B phase, are heated to 80 DEG C, insulation, as C phase;
(4)Under the conditions of controlling homogenizer rotating speed to be 12000r/min, the C phase of gained is slowly added in A phase, with
When with homogenizer continue homogenizing 3min;
(5)After homogenizing, it is cooled to 70 DEG C, use agitator instead and control speed of agitator to be stirred froth breaking for 200r/min;
(6)It is cooled to 45 DEG C after the completion of froth breaking, adds potassium sorbate, continue to control agitator speed to be stirred for 200r/min
Mix, to be cooled being cooled to after room temperature stops stirring;
(7)By step(6)It is ground as pasty mixture, fineness of the particles in the mixture input Multifunction colloid mill of gained
Less than 5 μm;
(8)By the pasty mixture after grinding, it is paste semi-finished product that input homogenizer carries out high speed strong stirring;
(9)Paste semi-finished product are carried out vacuum degassing process process, fill is sunscreen cream finished product.
Embodiment 2
Exocarpium Citri Grandises leaf naringin and Radix seu Folium Tosicodendri Delavayi glucoside sunscreen cream, are prepared from by the raw material of following weight fraction:Naringin and wild paint
Tree glycosides mixture 0.5%, Cera Flava 15%, ammonia ketone 1.0%, glycerol 10%, potassium sorbate 0.5%, balance of deionized water.
The preparation process of naringin and Radix seu Folium Tosicodendri Delavayi glucoside mixture is:
(1)Pluck Exocarpium Citri Grandises tender leaf to clean, the sun dries or puts in baking oven 60 DEG C dries to constant weight, pulverized 50 mesh sieves, and obtained leaf
Powder;
(2)Leaf powder is loaded in glass chromatography column, 95% food-grade ethanol makees extracting solution, in post, soak 60min, eluting liquor stream
Fast 100mL/h, collects eluent;
(3)The eluent of collection is carried out rotary evaporation in vacuo and is concentrated into paste;
(4)The concentrated solution of paste is transferred to separatory funnel, addition equivalent volumes petroleum ether extraction 3 times, removes upper liquid, obtain
Lower floor's extraction mixture;
(5)Lower floor's extraction mixture of gained is carried out rotary evaporation in vacuo be concentrated to dryness, washed with cold water 3 times, obtain Pericarpium Citri grandiss
Glycosides and Radix seu Folium Tosicodendri Delavayi glucoside mixture.
The preparation process of above-mentioned sunscreen cream is as follows:
(1)Solid Cera Flava will be taken to be heated to 85 DEG C, stirring and dissolving, as the insulation of A phase, standby;
(2)Glycerol is added in deionized water, as B phase, standby;
(3)Naringin and Radix seu Folium Tosicodendri Delavayi glucoside mixture are dissolved in B phase, are heated to 85 DEG C, insulation, as C phase;
(4)Under the conditions of controlling homogenizer rotating speed to be 15000r/min, the C phase of gained is slowly added in A phase, with
When with homogenizer continue homogenizing 3min;
(5)After homogenizing, it is cooled to 78 DEG C, use agitator instead and control speed of agitator to be stirred froth breaking for 300r/min;
(6)It is cooled to 45 DEG C after the completion of froth breaking, adds potassium sorbate, continue to control agitator speed to be stirred for 300r/min
Mix, to be cooled being cooled to after room temperature stops stirring;
(7)By step(6)It is ground as pasty mixture, fineness of the particles in the mixture input Multifunction colloid mill of gained
Less than 5 μm;
(8)By the pasty mixture after grinding, it is paste semi-finished product that input homogenizer carries out high speed strong stirring;
(9)Paste semi-finished product are carried out vacuum degassing process process, fill is sunscreen cream finished product.
Embodiment 3
Exocarpium Citri Grandises leaf naringin and Radix seu Folium Tosicodendri Delavayi glucoside sunscreen cream, are prepared from by the raw material of following weight fraction:Naringin and wild paint
Tree glycosides mixture 2.0%, Cera Flava 12%, ammonia ketone 0.4%, glycerol 8%, potassium sorbate 0.8%, balance of deionized water.
The preparation process of naringin and Radix seu Folium Tosicodendri Delavayi glucoside mixture is:
(1)Pluck Exocarpium Citri Grandises tender leaf to clean, the sun dries or puts in baking oven 60 DEG C dries to constant weight, pulverized 45 mesh sieves, and obtained leaf
Powder;
(2)Leaf powder is loaded in glass chromatography column, 95% food-grade ethanol makees extracting solution, in post, soak 70min, eluting liquor stream
Fast 95mL/h, collects eluent;
(3)The eluent of collection is carried out rotary evaporation in vacuo and is concentrated into paste;
(4)The concentrated solution of paste is transferred to separatory funnel, addition equivalent volumes petroleum ether extraction 4 times, removes upper liquid, obtain
Lower floor's extraction mixture;
(5)Lower floor's extraction mixture of gained is carried out rotary evaporation in vacuo be concentrated to dryness, washed with cold water 3 times, obtain Pericarpium Citri grandiss
Glycosides and Radix seu Folium Tosicodendri Delavayi glucoside mixture.
The preparation process of above-mentioned sunscreen cream is as follows:
(1)Solid Cera Flava will be taken to be heated to 75 DEG C, stirring and dissolving, as the insulation of A phase, standby;
(2)Glycerol is added in deionized water, as B phase, standby;
(3)Naringin and Radix seu Folium Tosicodendri Delavayi glucoside mixture are dissolved in B phase, are heated to 75 DEG C, insulation, as C phase;
(4)Under the conditions of controlling homogenizer rotating speed to be 20000r/min, the C phase of gained is slowly added in A phase, with
When with homogenizer continue homogenizing 3min;
(5)After homogenizing, it is cooled to 75 DEG C, use agitator instead and control speed of agitator to be stirred froth breaking for 500r/min;
(6)It is cooled to 45 DEG C after the completion of froth breaking, adds potassium sorbate, continue to control agitator speed to be stirred for 500r/min
Mix, to be cooled being cooled to after room temperature stops stirring;
(7)By step(6)It is ground as pasty mixture, fineness of the particles in the mixture input Multifunction colloid mill of gained
Less than 5 μm;
(8)By the pasty mixture after grinding, it is paste semi-finished product that input homogenizer carries out high speed strong stirring;
(9)Paste semi-finished product are carried out vacuum degassing process process, fill is sunscreen cream finished product.
Take above-mentioned containing naringin with Radix seu Folium Tosicodendri Delavayi glucoside mixture, be configured to, with ethanol, the solution that concentration is 20 μ g/mL, use ultraviolet
Spectrophotometer is analyzed, and the uv absorption spectra of gained is as shown in Figure 1.
As can be seen from Figure 1 naringin and Radix seu Folium Tosicodendri Delavayi glucoside are respectively provided with substantially in the range of ultraviolet wavelength 200~400nm
Ultraviolet absorption ability, absworption peak is not overlapping each other, particularly Radix seu Folium Tosicodendri Delavayi glucoside absorb main peak in long light wave scope, uv absorption
Scope is roomy, thus, illustrates that naringin and Radix seu Folium Tosicodendri Delavayi glucoside are a kind of safe efficient, wide spectrum natural plant sunscreen components, can
For in sun care preparationss.
The sunscreen product of two kinds of different brands and product of the present invention is taken to do ultraviolet suction peak spectrum and compare, result is shown in Fig. 2.Wherein
One of brand(Fig. 2, B, SPF (sun protection factor):SPF50+、PA+++)Ultra-violet absorption spectrum can be seen that this product 200 ~ 400
Uv absorption between nm is simultaneously uneven, and main absorption all concentrates between 280 ~ 330 nm and 200 ~ 240 nm.Brand it
Two(Fig. 2, C, SPF (sun protection factor):SPF50+、PA+++)Ultra-violet absorption spectrum it is known that this product is between 200 ~ 400 nm
Uv absorption very weak, main absorption all concentrates between 280 ~ 320 nm, and product of the present invention compares to UV Absorption
By force and uniformly.
Detection method according to People's Republic of China's industry index QB/T1857-1993 cosmetics is to product of the present invention
Sunscreen cream carries out physical and chemical index detection, the results are shown in Table 1.All refer to reference symbol standardization as seen from the table.
The assay of table 1 invention product sunscreen cream:
It is obvious to a person skilled in the art that the invention is not restricted to the details of above-mentioned one exemplary embodiment, and do not carrying on the back
In the case of the spirit or essential attributes of the present invention, the present invention can be realized in other specific forms.Therefore, no matter from which
From the point of view of a bit, embodiment all should be regarded as exemplary, and be nonrestrictive, the scope of the present invention will by appended right
Ask rather than described above limits, it is intended that all changes that will fall in the implication and scope of the equivalency of claim
Include in the present invention.Any reference in claim should not be considered as limiting involved claim.