CN106265487A - A kind of TANSHINONES emulsifiable paste process of preparing - Google Patents
A kind of TANSHINONES emulsifiable paste process of preparing Download PDFInfo
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- CN106265487A CN106265487A CN201610790491.3A CN201610790491A CN106265487A CN 106265487 A CN106265487 A CN 106265487A CN 201610790491 A CN201610790491 A CN 201610790491A CN 106265487 A CN106265487 A CN 106265487A
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- A61K9/06—Ointments; Bases therefor; Other semi-solid forms, e.g. creams, sticks, gels
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- A61K36/185—Magnoliopsida (dicotyledons)
- A61K36/53—Lamiaceae or Labiatae (Mint family), e.g. thyme, rosemary or lavender
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- A61K2236/33—Extraction of the material involving extraction with hydrophilic solvents, e.g. lower alcohols, esters or ketones
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Abstract
The invention provides a kind of TANSHINONES cream preparation method, comprise the following steps: red rooted salvia is added reflux, extract, in alcohol, decoction liquor concentrating under reduced pressure, obtains thick paste；By macroporous resin column on thick paste, water elution, ethanol elution, collect ethanol elution；Ethanol elution concentrating under reduced pressure, obtains dilute cream；Dilute cream room temperature stands, and filters, and precipitation is dried, and obtains TANSHINONES highly finished product；After distilled water is boiled, cooling, add triethanolamine, ethyl hydroxybenzoate and propylparaben mixing, obtain ointment aqueous phase；Or after distilled water is boiled, cooling, add propylene glycol, glycerol and sodium lauryl sulphate mixing, obtain ointment aqueous phase；After stearic acid, vaseline, octadecanol and liquid paraffin are mixed, heating；Add TANSHINONES highly finished product while stirring, then addition aqueous phase makes emulsifying while stirring, is down to room temperature, to obtain final product.The method technique is simple and convenient to operate, with low cost, be suitable to industrialized production.
Description
Technical field
The invention belongs to field of traditional Chinese, be specially a kind of TANSHINONES cream preparation method.
Background technology
Modern study thinks that the formation of pigmented spots is relatively big, because produced by hypophysis with pituitary secretion functional disorder relation
Melanin generation hormone can reduce the content of sulfenyl in skin makes pigmentation with increasing serum copper ions, forms color at face
Element speckle；And the traditional Chinese medical science thinks to be stagnation of QI due to depression of the liver, the stagnation of QI then blood stasis spotting.The generation of acne is main and hypersteatosis, hair follicle
The factors such as sebaceous gland duct blocking, antibacterial infection and inflammatory reaction are closely related.The androgen in descendant's body that adolesces is special
It is that the level of testosterone raises rapidly, promotes that sebaceous gland is grown and produces a large amount of sebum.The keratinization of pilosebaceous duct is different simultaneously
Often result in catheter blockage, dyssebacia, form horn plug i.e. micropowder thorn；SeborrheicaDermatitisAlso known as seborrheicaEczema, it is to send out
The chronic papulosquamous of one that life enriches position in sebaceous gland is struviteDermatosis, there is presently no good Therapeutic Method；
Chloasma is also referred to as chloasma hepaticum, and for the yellowish-brown pigmentation of face, many symmetrical butterflies are distributed in buccal, are more common in women, female in blood
Hormonal readiness height is main cause；Freckle women is more, and its numbers with age increases and is gradually increased, and is apt to occur in face, especially
Being nose and two cheeks, can involve the exposure portion such as neck, shoulder, the back of the hand, non-exposed position, without erythra, is damaged as shallow brown or crineous pin
Head size is to the big macule of Semen phaseoli radiati, circle, oval or irregular.It is dispersed in or cluster distribution, isolates and do not merge, no conscious sympton,
Summer is erythra color burn, increased number after Exposure to Sunlight, and winter then alleviates or disappears.
Radix Salviae Miltiorrhizae (Salvia milfirrhiza Bge.) is the dry root and rhizome of labiate, by chance has and invigorates blood circulation
Blood stasis dispelling effect thus reach effect of speckle dispelling.TANSHINONES is fat-soluble principle active component in Radix Salviae Miltiorrhizae, has confirmed Radix Salviae Miltiorrhizae
Ketone has and significantly reduces LPO and improve effect and antibacterial, antiinflammatory, the antioxygen of superoxide dismutase activity
The pharmacological actions widely such as change, estrogen-like effects, neuroprotective, have notable treatment to acne, seborrheic dermatitis, pigmentation
Effect.TANSHINONES is liposoluble substance, and wherein tanshinone ⅡA is practically insoluble in water, the dissolubility in water about 7 μ g/ml.The most such as
Fruit wants that skin splash etc. is had good therapeutic effect, needs to find one and TANSHINONES can be made to dissolve and rapid osmotic skin
Method.TANSHINONES is made ointment by the present invention, well solves this problem.According to the relevant pharmacological action of TANSHINONES,
All above disease had therapeutical effect, it is therefore desirable to explore suitable method and carry out symptomatic treatment with suitable dosage form.
Summary of the invention
Technical problem: in order to solve the defect of prior art, the invention provides a kind of TANSHINONES emulsifiable paste preparation side
Method.
Technical scheme: a kind of TANSHINONES cream preparation method that the present invention provides, comprises the following steps:
(1) TANSHINONES is extracted: red rooted salvia is added reflux, extract, in alcohol, decoction liquor concentrating under reduced pressure, obtains thick paste；
(2) purifying tanshinone: by macroporous resin column on thick paste, the water elution of 8-12 times amount, the ethanol of 10-15 times amount is washed
De-, collect ethanol elution；Ethanol elution concentrating under reduced pressure, obtains dilute cream；Dilute cream room temperature stands, and filters, and precipitation is dried, and obtains red
Ginseng ketone highly finished product；
(3) prepare ointment aqueous phase: after being boiled by distilled water, be cooled to 75-85 DEG C, add triethanolamine, nipalgin second
Ester and propylparaben mixing, obtain ointment aqueous phase；Or after being boiled by distilled water, it is cooled to 75-85 DEG C, adds the third two
Alcohol, glycerol and sodium lauryl sulphate mixing, obtain ointment aqueous phase；
(4) ointment oil phase is prepared: after stearic acid, vaseline, octadecanol and liquid paraffin being mixed, be heated to 80 DEG C；
(5) preparation of ointment: add TANSHINONES highly finished product, then limit in the ointment oil phase of step (4) while stirring
Stirring limit adds aqueous phase makes emulsifying, is cooled to 45-55 DEG C and stops stirring, is down to room temperature, to obtain final product.
In step (1), described alcohol is methanol or ethanol, and the mass percentage content of alcohol is 90-95%, and the quality of alcohol is red
6-8 times of ginseng quality of medicinal material, reflux temperature is 65-80 DEG C, and reflux, extract, number of times is 1-3 time, and reflux extracting time is 1-3h；Subtract
Push back shrinkage temperature and be 70-75 DEG C；Thick paste relative density is 1.2-1.5.
In step (2), described macroporous resin is D101 macroporous resin, D101-I macroporous resin or AB-8 type macroporous resin,
Fluid column is than for 1:(8～10)；The relative density of dilute cream is 1.0-1.2；TANSHINONES highly finished product are Tanshinone I IA, Tanshinone I IB, hidden
TANSHINONES and the mixture of Tanshinone I, wherein Tanshinone I IAContent is more than 45%, and cryptotanshinone content is more than 40%.
In step (3), the amount ratio of triethanolamine, ethyl hydroxybenzoate, propylparaben and water is (6-10) g:(0.6-
1.0) g:(0.06-0.10) g:300ml；The amount ratio of described propylene glycol, glycerol and sodium lauryl sulphate and water is (25-35)
G:(25-35) g:(2-8) g:500ml.
In step (4), the mass ratio of stearic acid, vaseline, octadecanol and liquid paraffin is (10-20): (20-30):
(10-20): (40-50).
In step (5), TANSHINONES amount is the 1-2% of ointment oil phase quality.
Beneficial effect: the TANSHINONES cream preparation method that the present invention provides, with Radix Salviae Miltiorrhizae as raw material, disposably obtains TANSHINONES
Emulsifiable paste, preparation technology is simple and convenient to operate, with low cost, is suitable to industrialized production, by clinic application to comedo, chloasma
Etc. there being good therapeutic effect.
The inventive method uses macroporous resin purification techniques after slightly extracting Radix Salviae Miltiorrhizae by ethanol, obtains the TANSHINONES that content is higher
Highly finished product, search out the suitable substrate carrier as TANSHINONES, the form of application ointment simultaneously, enable TANSHINONES to make
For suitable dosage form, quickly penetrate into skin, can quickly absorb, disease is had therapeutic effect.Western medicine acne, fat at present
The dermatosiss such as property dermatitis of overflowing easily cause allergic reaction, and effect is not the most preferable, and the present invention is through using above-mentioned disease
Having good curative effect, application extensively has wide DEVELOPMENT PROSPECT.
Detailed description of the invention
Embodiment 1
(1) extract TANSHINONES: the red rooted salvia in the place of production, Sichuan is cut into chunks, add 6 times of quality 95% ethanol in 80 DEG C
Reflux, extract, 1h, filtering residue repetitive operation 1 time, 70 DEG C of concentrating under reduced pressure of decoction liquor, obtain thick paste, thick paste relative density is 1.3；
(2) purifying tanshinone: by D101 macroporous resin on thick paste, loading fluid column than for 1:8, the water elution of 10 times amount, 15
95% ethanol elution of times amount, collects ethanol elution；Ethanol elution concentrating under reduced pressure, obtains dilute cream, and the relative density of dilute cream is
1.1；Dilute cream room temperature stands, and filters, and precipitation is dried, and obtains TANSHINONES highly finished product；Wherein, TANSHINONES highly finished product are Tanshinone I IA、
Tanshinone I IB, cryptotanshinone and the mixture of Tanshinone I, wherein Tanshinone I IAContent is more than 45%, and cryptotanshinone content exists
More than 40%；
(3) preparing ointment aqueous phase: after being boiled by distilled water, be cooled to 80 DEG C, addition amount ratio is 8g:0.8g:
The triethanolamine of 0.08g:300ml, ethyl hydroxybenzoate and propylparaben mixing, obtain ointment aqueous phase；
(4) ointment oil phase is prepared: be the stearic acid of 15g:25g:15g:45g, vaseline, octadecanol and liquid by mass ratio
After paraffin body mixing, it is heated to 80 DEG C；
(5) preparation of ointment: add TANSHINONES highly finished product, Radix Salviae Miltiorrhizae while stirring in the ointment oil phase of step (4)
The quality of ketone highly finished product is the 2% of ointment oil phase quality, then addition aqueous phase makes emulsifying while stirring, is cooled to 50 DEG C of stoppings and stirring
Mix, be down to room temperature, to obtain final product.
Its active constituent content of the product drawn (in terms of tanshinone ⅡA and cryptotanshinone) and retention rate are shown in Table 1.
Table 1
Embodiment 2
TANSHINONES cream preparation method, comprises the following steps:
(1) extract TANSHINONES: cut into chunks by the red rooted salvia in the places of production such as Shandong, add 65-in 93% ethanol of 7 times of quality
80 DEG C of reflux, extract, 1h, filtering residue repetitive operation 1 time, 75 DEG C of concentrating under reduced pressure of decoction liquor, obtain thick paste, thick paste relative density is 1.2；
(2) purifying tanshinone: by D101-I macroporous resin on thick paste, loading fluid column than for 1:9, the water elution of 10 times amount,
95% ethanol elution of 13 times amount, collects ethanol elution；Ethanol elution concentrating under reduced pressure, obtains dilute cream, the relative density of dilute cream
It is 1.1；Dilute cream room temperature stands, and filters, and precipitation is dried, and obtains TANSHINONES highly finished product；Wherein, TANSHINONES highly finished product are TANSHINONES
IIA, Tanshinone I IB, cryptotanshinone and the mixture of Tanshinone I, wherein Tanshinone I IAContent is more than 45%, and cryptotanshinone contains
Amount is more than 40%；
(3) preparing ointment aqueous phase: after being boiled by distilled water, be cooled to 80 DEG C, addition amount ratio is 30g:30:5:
The propylene glycol of 500ml, glycerol and sodium lauryl sulphate mixing, obtain ointment aqueous phase；
(4) ointment oil phase is prepared: be the stearic acid of 15g:25g:15g:45g, vaseline, octadecanol and liquid by mass ratio
After paraffin body mixing, it is heated to 80 DEG C；
(5) preparation of ointment: add TANSHINONES highly finished product, Radix Salviae Miltiorrhizae while stirring in the ointment oil phase of step (4)
The quality of ketone highly finished product is the 1.5% of ointment oil phase quality, then addition aqueous phase makes emulsifying while stirring, is cooled to 50 DEG C of stoppings
Stirring, is down to room temperature, to obtain final product.
Its active constituent content of the product drawn (in terms of tanshinone ⅡA and cryptotanshinone) and retention rate are shown in Table 2.
Table 2
Embodiment 3
TANSHINONES cream preparation method, comprises the following steps:
(1) extract TANSHINONES: the red rooted salvia in the place of production, Sichuan is cut into chunks, add 8 times of quality 90% ethanol in 80 DEG C
Reflux, extract, 1h, filtering residue repetitive operation 1 time, 75 DEG C of concentrating under reduced pressure of decoction liquor, obtain thick paste, thick paste relative density is 1.4；
(2) purifying tanshinone: by AB-8 type macroporous resin on thick paste, loading fluid column than for 1:10, the water elution of 10 times amount,
95% ethanol elution of 10 times amount, collects ethanol elution；Ethanol elution concentrating under reduced pressure, obtains dilute cream, the relative density of dilute cream
It is 1.1；Dilute cream room temperature stands, and filters, and precipitation is dried, and obtains TANSHINONES highly finished product；Wherein, TANSHINONES highly finished product are TANSHINONES
IIA, Tanshinone I IB, cryptotanshinone and the mixture of Tanshinone I, wherein Tanshinone I IAContent is more than 45%, and cryptotanshinone contains
Amount is more than 40%；
(3) preparing ointment aqueous phase: after being boiled by distilled water, be cooled to 80 DEG C, addition amount ratio is 8g:0.8g:
The triethanolamine of 0.08g:300ml, ethyl hydroxybenzoate and propylparaben mixing, obtain ointment aqueous phase；
(4) ointment oil phase is prepared: be the stearic acid of 15:25:15:45, vaseline, octadecanol and liquid stone by mass ratio
After wax mixing, it is heated to 80 DEG C；
(5) preparation of ointment: add TANSHINONES highly finished product, Radix Salviae Miltiorrhizae while stirring in the ointment oil phase of step (4)
The quality of ketone highly finished product is the 1% of ointment oil phase quality, then addition aqueous phase makes emulsifying while stirring, is cooled to 50 DEG C of stoppings and stirring
Mix, be down to room temperature, to obtain final product.
Its active constituent content of the product drawn (in terms of tanshinone ⅡA and cryptotanshinone) and retention rate are shown in Table 3.
Table 3
Embodiment 4
TANSHINONES cream preparation method, comprises the following steps:
(1) extract TANSHINONES: the red rooted salvia in the place of production, Sichuan is cut into chunks, add 7 times of quality 95% ethanol in 80 DEG C
Reflux, extract, 1h, filtering residue repetitive operation 1 time, 73 DEG C of concentrating under reduced pressure of decoction liquor, obtain thick paste, thick paste relative density is 1.2；
(2) purifying tanshinone: by AB-8 type macroporous resin on thick paste, loading fluid column than for 1:9, the water elution of 10 times amount,
95% ethanol elution of 12 times amount, collects ethanol elution；Ethanol elution concentrating under reduced pressure, obtains dilute cream, the relative density of dilute cream
It is 1.0；Dilute cream room temperature stands, and filters, and precipitation is dried, and obtains TANSHINONES highly finished product；Wherein, TANSHINONES highly finished product are TANSHINONES
IIA, Tanshinone I IB, cryptotanshinone and the mixture of Tanshinone I, wherein Tanshinone I IAContent is more than 45%, and cryptotanshinone contains
Amount is more than 40%；
(3) preparing ointment aqueous phase: after being boiled by distilled water, be cooled to 80 DEG C, addition amount ratio is 30g:30g:5g:
The propylene glycol of 500ml, glycerol and sodium lauryl sulphate mixing, obtain ointment aqueous phase；
(4) ointment oil phase is prepared: be the stearic acid of 15:25:15:45, vaseline, octadecanol and liquid stone by mass ratio
After wax mixing, it is heated to 80 DEG C；
(5) preparation of ointment: add TANSHINONES highly finished product, Radix Salviae Miltiorrhizae while stirring in the ointment oil phase of step (4)
The quality of ketone highly finished product is the 2% of ointment oil phase quality, then addition aqueous phase makes emulsifying while stirring, is cooled to 50 DEG C of stoppings and stirring
Mix, be down to room temperature, to obtain final product.
Its active constituent content of the product drawn (in terms of tanshinone ⅡA and cryptotanshinone) and retention rate are shown in Table 4.
Table 4
Embodiment 5
TANSHINONES cream preparation method, comprises the following steps:
(1) extract TANSHINONES: the red rooted salvia in the place of production, Sichuan is cut into chunks, add 8 times of quality 95% ethanol in 80 DEG C
Reflux, extract, 1h, filtering residue repetitive operation 1 time, 70 DEG C of concentrating under reduced pressure of decoction liquor, obtain thick paste, thick paste relative density is 1.2；
(2) purifying tanshinone: by AB-8 type macroporous resin on thick paste, loading fluid column than for 1:8, the water elution of 10 times amount,
95% ethanol elution of 13 times amount, collects ethanol elution；Ethanol elution concentrating under reduced pressure, obtains dilute cream, the relative density of dilute cream
It is 1.2；Dilute cream room temperature stands, and filters, and precipitation is dried, and obtains TANSHINONES highly finished product；Wherein, TANSHINONES highly finished product are TANSHINONES
IIA, Tanshinone I IB, cryptotanshinone and the mixture of Tanshinone I, wherein Tanshinone I IAContent is more than 45%, and cryptotanshinone contains
Amount is more than 40%；
(3) preparing ointment aqueous phase: after being boiled by distilled water, be cooled to 75-85 DEG C, addition amount ratio is 30g:30g:
The triethanolamine of 5g:500ml, ethyl hydroxybenzoate and propylparaben mixing, obtain ointment aqueous phase；
(4) ointment oil phase is prepared: be the stearic acid of 15:25:15:45, vaseline, octadecanol and liquid stone by mass ratio
After wax mixing, it is heated to 80 DEG C；
(5) preparation of ointment: add TANSHINONES highly finished product, Radix Salviae Miltiorrhizae while stirring in the ointment oil phase of step (4)
The quality of ketone highly finished product is the 2% of ointment oil phase quality, then addition aqueous phase makes emulsifying while stirring, is cooled to 50 DEG C of stoppings and stirring
Mix, be down to room temperature, to obtain final product.
Its active constituent content of the product drawn (in terms of tanshinone ⅡA and cryptotanshinone) and retention rate are shown in Table 5.
Table 5
Embodiment 6
TANSHINONES cream preparation method, comprises the following steps:
(1) extract TANSHINONES: the red rooted salvia in the place of production, Sichuan is cut into chunks, add 6 times of quality 95% methanol in 65 DEG C
Reflux, extract, 3h, 70 DEG C of concentrating under reduced pressure of decoction liquor, obtain thick paste, thick paste relative density is 1.2；
(2) purifying tanshinone: by D101 macroporous resin on thick paste, loading fluid column than for 1:8, the water elution of 8 times amount, 10 times
95% ethanol elution of amount, collects ethanol elution；Ethanol elution concentrating under reduced pressure, obtains dilute cream, and the relative density of dilute cream is
1.0；Dilute cream room temperature stands, and filters, and precipitation is dried, and obtains TANSHINONES highly finished product；Wherein, TANSHINONES highly finished product are Tanshinone I IA、
Tanshinone I IB, cryptotanshinone and the mixture of Tanshinone I, wherein Tanshinone I IAContent is more than 45%, and cryptotanshinone content exists
More than 40%；
(3) preparing ointment aqueous phase: after being boiled by distilled water, be cooled to 85 DEG C, addition amount ratio is 10g:0.6g:
The triethanolamine of 0.10g:300ml, ethyl hydroxybenzoate and propylparaben mixing, obtain ointment aqueous phase；
(4) ointment oil phase is prepared: be the stearic acid of 20:30:10:40, vaseline, octadecanol and liquid stone by mass ratio
After wax mixing, it is heated to 80 DEG C；
(5) preparation of ointment: add TANSHINONES highly finished product, Radix Salviae Miltiorrhizae while stirring in the ointment oil phase of step (4)
The quality of ketone highly finished product is the 1% of ointment oil phase quality, then addition aqueous phase makes emulsifying while stirring, is cooled to 55 DEG C of stoppings and stirring
Mix, be down to room temperature, to obtain final product.
Its active constituent content of the product drawn (in terms of tanshinone ⅡA and cryptotanshinone) and retention rate are shown in Table 6.
Table 6
Embodiment 7
TANSHINONES cream preparation method, comprises the following steps:
(1) extract TANSHINONES: the red rooted salvia in the place of production, Sichuan is cut into chunks, add 8 times of quality 90% methanol in 70 DEG C
Reflux, extract, 1h, filtering residue repetitive operation repeats 1-3 time, and 75 DEG C of concentrating under reduced pressure of decoction liquor obtain thick paste, and thick paste relative density is 1.5；
(2) purifying tanshinone: by D101-I macroporous resin on thick paste, loading fluid column than for 1:10, the water elution of 12 times amount,
95% ethanol elution of 15 times amount, collects ethanol elution；Ethanol elution concentrating under reduced pressure, obtains dilute cream, the relative density of dilute cream
It is 1.2；Dilute cream room temperature stands, and filters, and precipitation is dried, and obtains TANSHINONES highly finished product；Wherein, TANSHINONES highly finished product are TANSHINONES
IIA, Tanshinone I IB, cryptotanshinone and the mixture of Tanshinone I, wherein Tanshinone I IAContent is more than 45%, and cryptotanshinone contains
Amount is more than 40%；
(3) preparing ointment aqueous phase: after being boiled by distilled water, be cooled to 75 DEG C, addition amount ratio is 6g:1.0g:
The triethanolamine of 0.06g:300ml, ethyl hydroxybenzoate and propylparaben mixing, obtain ointment aqueous phase；
(4) ointment oil phase is prepared: be the stearic acid of 10:20:20:50, vaseline, octadecanol and liquid stone by mass ratio
After wax mixing, it is heated to 80 DEG C；
(5) preparation of ointment: add TANSHINONES highly finished product, Radix Salviae Miltiorrhizae while stirring in the ointment oil phase of step (4)
The quality of ketone highly finished product is the 2% of ointment oil phase quality, then addition aqueous phase makes emulsifying while stirring, is cooled to 45 DEG C of stoppings and stirring
Mix, be down to room temperature, to obtain final product.
Its active constituent content of the product drawn (in terms of tanshinone ⅡA and cryptotanshinone) and retention rate are shown in Table 7.
Table 7
Embodiment 8
TANSHINONES cream preparation method, comprises the following steps:
(1) extract TANSHINONES: the red rooted salvia in the place of production, Sichuan is cut into chunks, add 6 times of quality 95% methanol in 65 DEG C
Reflux, extract, 3h, 70 DEG C of concentrating under reduced pressure of decoction liquor, obtain thick paste, thick paste relative density is 1.2；
(2) purifying tanshinone: by D101 macroporous resin on thick paste, loading fluid column than for 1:8, the water elution of 8 times amount, 10 times
95% ethanol elution of amount, collects ethanol elution；Ethanol elution concentrating under reduced pressure, obtains dilute cream, and the relative density of dilute cream is
1.0；Dilute cream room temperature stands, and filters, and precipitation is dried, and obtains TANSHINONES highly finished product；Wherein, TANSHINONES highly finished product are Tanshinone I IA、
Tanshinone I IB, cryptotanshinone and the mixture of Tanshinone I, wherein Tanshinone I IAContent is more than 45%, and cryptotanshinone content exists
More than 40%；
(3) preparing ointment aqueous phase: after being boiled by distilled water, be cooled to 75 DEG C, addition amount ratio is 25g:35g:2g:
The propylene glycol of 500ml, glycerol and sodium lauryl sulphate mixing, obtain ointment aqueous phase；
(4) ointment oil phase is prepared: be the stearic acid of 20:30:10:40, vaseline, octadecanol and liquid stone by mass ratio
After wax mixing, it is heated to 80 DEG C；
(5) preparation of ointment: add TANSHINONES highly finished product, Radix Salviae Miltiorrhizae while stirring in the ointment oil phase of step (4)
The quality of ketone highly finished product is the 1% of ointment oil phase quality, then addition aqueous phase makes emulsifying while stirring, is cooled to 55 DEG C of stoppings and stirring
Mix, be down to room temperature, to obtain final product.
Its active constituent content of the product drawn (in terms of tanshinone ⅡA and cryptotanshinone) and retention rate are shown in Table 8.
Table 8
Embodiment 9
TANSHINONES cream preparation method, comprises the following steps:
(1) extract TANSHINONES: the red rooted salvia in the place of production, Sichuan is cut into chunks, add 8 times of quality 90% methanol in 70 DEG C
Reflux, extract, 1h, filtering residue repetitive operation repeats 1-3 time, and 75 DEG C of concentrating under reduced pressure of decoction liquor obtain thick paste, and thick paste relative density is 1.5；
(2) purifying tanshinone: by D101-I macroporous resin on thick paste, loading fluid column than for 1:10, the water elution of 12 times amount,
95% ethanol elution of 15 times amount, collects ethanol elution；Ethanol elution concentrating under reduced pressure, obtains dilute cream, the relative density of dilute cream
It is 1.2；Dilute cream room temperature stands, and filters, and precipitation is dried, and obtains TANSHINONES highly finished product；Wherein, TANSHINONES highly finished product are TANSHINONES
IIA, Tanshinone I IB, cryptotanshinone and the mixture of Tanshinone I, wherein Tanshinone I IAContent is more than 45%, and cryptotanshinone contains
Amount is more than 40%；
(3) preparing ointment aqueous phase: after being boiled by distilled water, be cooled to 85 DEG C, addition amount ratio is 35g:25g:8g:
The propylene glycol of 500ml, glycerol and sodium lauryl sulphate mixing, obtain ointment aqueous phase；
(4) ointment oil phase is prepared: be the stearic acid of 10:20:20:50, vaseline, octadecanol and liquid stone by mass ratio
After wax mixing, it is heated to 80 DEG C；
(5) preparation of ointment: add TANSHINONES highly finished product, Radix Salviae Miltiorrhizae while stirring in the ointment oil phase of step (4)
The quality of ketone highly finished product is the 2% of ointment oil phase quality, then addition aqueous phase makes emulsifying while stirring, is cooled to 45 DEG C of stoppings
Stirring, is down to room temperature, to obtain final product.
Its active constituent content of the product drawn (in terms of tanshinone ⅡA and cryptotanshinone) and retention rate are shown in Table 9.
Table 9
Zoopery
Skin Irritation Test: shave off the hair about 3.0 of rabbit back2, allow rabbit rest 24h, the by the time thorn at shaving position
Swash recovery from illness, take 0.6g this product uniformly rabbit back be coated with straticulation, observer's rabbit skin after 36h, do not find erythema, edema,
The phenomenons such as rash block.
Eye mucosa assay method: eyelid coating 0.30g this product in rabbit eyes, every 0.5h observation 1 time in 2h, after 36h again
Observe 1 time, all do not find a conjunctiva occur edema, hyperemia, shed tears, photophobia and the uneasy phenomenon of disturbance occur.
Hypersensitive test: shave off the hair of Cavia porcellus back, after 24h on shaving administrative division map 0.15g this product, for three days on end, the 14th
It repeats once, with sensitization.It is administered again after 14 days to excite anaphylaxis.Remove medicine after 8h, respectively 24h, 36h,
48h, 72h observe dermoreaction, all without red and swollen, edema and other skin allergies.
Comparative example: compare with TANSHINONES emulsifiable paste and dewrinkling spot-eliminating cream, be specifically shown in Table 10.
Table 10
The present invention have found a kind of exquisite TANSHINONES the method making ointment, and this dosage form is to comedo, seborrhea
Property dermatitis, pigmentation etc. there is good curative effect, solve patient's puzzlement disease for many years.The main contribution of this technology is exactly
Exquisite TANSHINONES content can reach more than 40%, and make ointment and bring benefit to the people, and has treated the relevant disease of stagnation of QI due to depression of the liver etc.
Disease, therefore this technology has clinical value very much.
The present invention concrete technical scheme required for protection, is not limited to the concrete of technical scheme expressed by above-described embodiment
Combination, including its all of assembled scheme.
Claims (6)
1. a TANSHINONES cream preparation method, it is characterised in that: comprise the following steps:
(1) TANSHINONES is extracted: red rooted salvia is added reflux, extract, in alcohol, decoction liquor concentrating under reduced pressure, obtains thick paste；
(2) purifying tanshinone: by macroporous resin column on thick paste, the water elution of 8-12 times amount, the ethanol elution of 10-15 times amount, receive
Collection ethanol elution；Ethanol elution concentrating under reduced pressure, obtains dilute cream；Dilute cream room temperature stands, and filters, and precipitation is dried, and obtains TANSHINONES
Highly finished product；
(3) prepare ointment aqueous phase: after being boiled by distilled water, be cooled to 75-85 DEG C, add triethanolamine, ethyl hydroxybenzoate and
Propylparaben mixes, and obtains ointment aqueous phase；Or after being boiled by distilled water, it is cooled to 75-85 DEG C, adds propylene glycol, sweet
Oil and sodium lauryl sulphate mix, and obtain ointment aqueous phase；
(4) ointment oil phase is prepared: after stearic acid, vaseline, octadecanol and liquid paraffin being mixed, be heated to 80 DEG C；
(5) preparation of ointment: add TANSHINONES highly finished product, then limit stirring in the ointment oil phase of step (4) while stirring
Limit adds aqueous phase makes emulsifying, is cooled to 45-55 DEG C and stops stirring, is down to room temperature, to obtain final product.
A kind of TANSHINONES cream preparation method the most according to claim 1, it is characterised in that: in step (1), described alcohol is
Methanol or ethanol, the mass percentage content of alcohol is 90-95%, and the quality of alcohol is 6-8 times of red rooted salvia quality, reflux temperature
For 65-80 DEG C, reflux, extract, number of times is 1-3 time, and reflux extracting time is 1-3h；Recovered under reduced pressure temperature is 70-75 DEG C；Thick paste phase
It is 1.2-1.5 to density.
A kind of TANSHINONES cream preparation method the most according to claim 1, it is characterised in that: in step (2), described macropore
Resin is D101 macroporous resin, D101-I macroporous resin or AB-8 type macroporous resin, and fluid column is than for 1:(8～10)；The phase of dilute cream
It is 1.0-1.2 to density；TANSHINONES highly finished product are Tanshinone I IA, Tanshinone I IB, cryptotanshinone and the mixture of Tanshinone I, its
Middle Tanshinone I IAContent is more than 45%, and cryptotanshinone content is more than 40%.
A kind of TANSHINONES cream preparation method the most according to claim 1, it is characterised in that: in step (3), three ethanol
The amount ratio of amine, ethyl hydroxybenzoate, propylparaben and water is (6-10) g:(0.6-1.0) g:(0.06-0.10) g:300ml；
The amount ratio of described propylene glycol, glycerol and sodium lauryl sulphate and water is (25-35) g:(25-35) g:(2-8) g:500ml.
A kind of TANSHINONES cream preparation method the most according to claim 1, it is characterised in that: in step (4), stearic acid,
The mass ratio of vaseline, octadecanol and liquid paraffin is (10-20): (20-30): (10-20): (40-50).
A kind of TANSHINONES cream preparation method the most according to claim 1, it is characterised in that: in step (5), TANSHINONES amount
1-2% for ointment oil phase quality.
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Citations (3)
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| CN1670019A (en) * | 2004-03-17 | 2005-09-21 | 天津天士力现代中药资源有限公司 | Process for extracting tanshinone |
| CN102973653A (en) * | 2012-12-17 | 2013-03-20 | 颜晓文 | Preparation method of tanshinone extract and water soluble substance thereof |
| CN105520904A (en) * | 2014-09-30 | 2016-04-27 | 陈彦 | Cream preparation method |
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2016
- 2016-08-31 CN CN201610790491.3A patent/CN106265487A/en active Pending
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1670019A (en) * | 2004-03-17 | 2005-09-21 | 天津天士力现代中药资源有限公司 | Process for extracting tanshinone |
| CN102973653A (en) * | 2012-12-17 | 2013-03-20 | 颜晓文 | Preparation method of tanshinone extract and water soluble substance thereof |
| CN105520904A (en) * | 2014-09-30 | 2016-04-27 | 陈彦 | Cream preparation method |
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| 刘文彬，等: "外用丹参酮乳膏抗痤疮药效及机制", 《中国实验方剂学杂志》 * |
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Application publication date: 20170104 |