CN109550006A - The impurity-removing method of clean yin itching-relieving lotion - Google Patents

The impurity-removing method of clean yin itching-relieving lotion Download PDF

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CN109550006A
CN109550006A CN201811369191.3A CN201811369191A CN109550006A CN 109550006 A CN109550006 A CN 109550006A CN 201811369191 A CN201811369191 A CN 201811369191A CN 109550006 A CN109550006 A CN 109550006A
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itching
sample
impurity
relieving lotion
solution
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赵子剑
罗正红
严丽莹
梁玉兰
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Huaihua University
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Huaihua University
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Abstract

The present invention relates to a kind of impurity-removing methods of clean negative itching-relieving lotion.The impurity-removing method of the clean negative itching-relieving lotion, comprising the following steps: after clean negative itching-relieving lotion centrifugation, after filtering with microporous membrane, filtrate is completed into removal of impurities using ultrafiltration membrance filter.The impurity-removing method of above-mentioned clean negative itching-relieving lotion, several impurity-removing methods of integrated use, it is preferred that the removal of impurities production technology of clean negative itching-relieving lotion, improve finished product clarity, increase the stability of patent medicine, it improves dope existing for former patent medicine to be sunken to bottom of bottle and be hung on a bottle wall, for inlet tube due to resulting in blockage after spraying use is repeated several times, medical fluid is not easy the shortcomings that spraying in spray bottle packaging.

Description

The impurity-removing method of clean yin itching-relieving lotion
Technical field
The present invention relates to Chinese medicine extract process fields, more particularly to the impurity-removing method of clean negative itching-relieving lotion.
Background technique
Clean yin itching-relieving lotion is by kuh-seng, folium panacis japonici cum caule, frutus cnidii, Cortex Phellodendri, radix paeoniae rubra, Chinese prickly ash, climbing groundsel, smilax, Radix Glycyrrhizae, Xu Long minister in ancient times, polygonum cuspidate, 12 taste traditional Chinese medicine extraction of menthol are made, and have the effect of clearing heat and detoxicating, nourishing yin to moisten dryness, dispelling wind and arresting itching, to face Pudendal pruritus compound Chinese patent medicine caused by bed true medicable treatment damp invasion of lower energizer, liver-kidney yin deficiency vaginitis.
Clean yin itching-relieving lotion original production process is alcohol deposition method technique.The basic principle of common alcohol deposition method is using in Chinese medicine Part effective component be not only dissolved in water but also be dissolved in the property of alcohol, removed using alcohol deposition method and be partially insoluble in the component of ethyl alcohol as more Sugar, protein etc., to achieve the purpose that fine work is made.But it is found in clinical use, after existing patent medicine storage, there are dopes The problem of being sunken to bottom of bottle and being hung on bottle wall, and inlet tube is produced in spray bottle packaging due to causing after spraying use is repeated several times Blocking, medical fluid are not easy the shortcomings that spraying.
Summary of the invention
Based on this, it is necessary to aiming at the problem that impurity effect storage and production of clean negative itching-relieving lotion, provide a kind of clean yin The impurity-removing method of itching-relieving lotion.
A kind of impurity-removing method of clean negative itching-relieving lotion, comprising the following steps:
After clean negative itching-relieving lotion centrifugation, after filtering with microporous membrane, filtrate is completed into removal of impurities using ultrafiltration membrance filter.
Further, it is 1500~3000 turns/min that centrifugal condition, which is centrifugal rotational speed, and when centrifugation is 15~30 minutes a length of.
Further, the aperture of miillpore filter is 0.45-0.22 microns, and it is 0.05-0.15MPa, stream that filtering, which applies pressure, Fast 0.1-0.5m/s, the aperture of ultrafiltration membrane are 2-50 nanometers, and it is 0.01-0.1MPa, flow velocity 0.1-0.5m/s that filtering, which applies pressure,.
The impurity-removing method of above-mentioned clean negative itching-relieving lotion, several impurity-removing methods of integrated use, preferably clean negative itching-relieving lotion Clean production technology, improves finished product clarity, increases the stability of patent medicine, improves dope existing for former patent medicine and be sunken to Bottom of bottle and it is hung on a bottle wall, due to resulting in blockage after spraying use is repeated several times, medical fluid is not easy to spray inlet tube in spray bottle packaging The shortcomings that.
Detailed description of the invention
Fig. 1 is the separating technology flow chart of sample A, B, C, D of clean negative itching-relieving lotion water；
The Cortex Phellodendri TLC that Fig. 2 is sample A schemes；
The Cortex Phellodendri TLC that Fig. 3 is sample B schemes；
The Cortex Phellodendri TLC that Fig. 4 is sample C schemes；
The Cortex Phellodendri TLC that Fig. 5 is sample D schemes；
The radix paeoniae rubra TLC that Fig. 6 is sample A schemes；
The radix paeoniae rubra TLC that Fig. 7 is sample B schemes；
The radix paeoniae rubra TLC that Fig. 8 is sample C schemes；
The radix paeoniae rubra TLC that Fig. 9 is sample D schemes；
The polygonum cuspidate TLC that Figure 10 is sample A schemes；
The polygonum cuspidate TLC that Figure 11 is sample B schemes；
The polygonum cuspidate TLC that Figure 12 is sample C schemes；
The polygonum cuspidate TLC that Figure 13 is sample D schemes；
The menthol TLC that Figure 14 is sample A schemes；
The menthol TLC that Figure 15 is sample B schemes；
The menthol TLC that Figure 16 is sample C schemes；
The menthol TLC that Figure 17 is sample D schemes；
The folium panacis japonici cum caule TLC that Figure 18 is sample A schemes；
The folium panacis japonici cum caule TLC that Figure 19 is sample B schemes；
The folium panacis japonici cum caule TLC that Figure 20 is sample C schemes；
The folium panacis japonici cum caule TLC that Figure 21 is sample D schemes；
The Radix Glycyrrhizae TLC that Figure 22 is sample A schemes；
The Radix Glycyrrhizae TLC that Figure 23 is sample B schemes；
The Radix Glycyrrhizae TLC that Figure 24 is sample C schemes；
The Radix Glycyrrhizae TLC that Figure 25 is sample D schemes.
Specific embodiment
In order to make the foregoing objectives, features and advantages of the present invention clearer and more comprehensible, with reference to the accompanying drawing to the present invention Specific embodiment be described in detail.Many details are explained in the following description in order to fully understand this hair It is bright.But the invention can be embodied in many other ways as described herein, those skilled in the art can be not Similar improvement is done in the case where violating intension of the present invention, therefore the present invention is not limited to the specific embodiments disclosed below.
A kind of impurity-removing method of clean negative itching-relieving lotion, comprising the following steps:
After clean negative itching-relieving lotion centrifugation, after filtering with microporous membrane, filtrate is completed into removal of impurities using ultrafiltration membrance filter.
Further, it is 1500~3000 turns/min that centrifugal condition, which is centrifugal rotational speed, and when centrifugation is 15~30 minutes a length of.Turn Number is excessively high, and centrifugal force is too big, will cause the loss of effective component；Revolution is too low, and impurity-eliminating effect is not achieved.Centrifugation time is too long, Uneconomical, the time is too short, then impurity-eliminating effect is not achieved.
Further, the aperture of miillpore filter is 0.45-0.22 microns, and it is 0.05-0.15MPa, stream that filtering, which applies pressure, Fast 0.1-0.5m/s, the aperture of ultrafiltration membrane are 2-50 nanometers, and it is 0.01-0.1MPa, flow velocity 0.1-0.5m/s that filtering, which applies pressure,.
Filter sizes are excessive, and impurity-eliminating effect is not achieved, and filter sizes are too small, can retain effective component and filter only medical fluid, It is uneconomical.Flow velocity is excessively slow, uneconomical, and flow velocity is too fast, then impurity-eliminating effect is not achieved.
Embodiment
The membrane filtration processes of washing lotion are studied
The production technology experimental design and explanation of 1.1 clean negative itching-relieving lotion modifications
This experiment omits former washing lotion and production technology early period is concentrated, and studies concentrate later-period purification technique, concentrate It is provided by Huaihua Zhenghao Pharmaceutical Co., Ltd..
1.1.1 the preparation of sample
(1) taking concentrate 300mL is sample A.As shown in Figure 1.
(2) taking 24 hours concentrate V1=300mL of refrigeration is medical fluid I.Claim its quality m=368.9g.Ethyl alcohol is added to make alcohol-containing Amount is 30%, and (ethyl alcohol 158.1g) is uniformly mixed.It stands more than for 24 hours.After recycling ethyl alcohol, alcohol precipitation supernatant volume V2= 263mL is sample D.As shown in Figure 1.
(3) refrigerating and taking within 24 hours concentrate V1=500mL is medical fluid II, obtains medical fluid body after the filtering of UF membrane experimental provision Product V2=485mL, is sampled as sample B.As shown in Figure 1.
(4) concentrate 300mL is taken, sample volume 300mL after centrifugation, then medicine liquid volume is obtained after membrane separation device filters 229mL is sampled as sample C.As shown in Figure 1.
The measurement of 2 sample quality evaluation indexes
2.1 product yield
A certain amount of medical fluid I is taken, its volume V1 is recorded.After corresponding process, its volume V2 is recorded.Sample finished product is received Rate α is V2/V1 × 100%.Then have:
αB=485/500 × 100%=97%
αC=285/300 × 100%=95%
αD=263/300 × 100%=88%
2.2 clarity
Using lamp test.Sample to be tested is taken, container outer wall is cleaned, outer wall dry cleansing is kept, is centrally placed, through clear and bright Somascope detection is spent, sample A, B, C, D are complied with standard without visible foreign matters.
2.3 solid content
Separately sampled product A, B, C, D are measured using refractometry.Before test sample, first with distilled water calibration refractometer reading, make 0 scale is kept after refractometer calibration.Then net distilled water is wiped with lens wiping paper, takes and shakes up the drop of sample drop one in abbe's refractometer plane On, cover upper cover, constant temperature (20 DEG C) 30s, adjusting knob, until observing that light and shade cut-off rule appears in Shi Jinhang on cross crunode Sample temperature when reading, while recording measurement, as a result such as following table 3.1.
Data record:
3.1 soluble solid content of table (20 DEG C)
The Qualitive test of 2.4 technique finished products
2.4.1 the thin layer of Cortex Phellodendri identifies
Sample solution 10ml is measured in ceramic whiteware evaporating dish, places it on 80 DEG C of HH digital display thermostat water baths and steams to close Dry, then 5~10min of ultrasonic treatment in ultrasonic cleaner is set in the dissolution of residue obtained plus proper amount of methanol, rear to take out filtration, institute Obtaining filtrate is test solution.
Cortex Phellodendri control medicinal material 0.4g is taken, methanol 20mL is measured, sets in a round bottom flask, be heated to reflux in being heated to reflux device 15min then takes out, and by the cooling filtration of remaining liq, gained filtrate adds methanol to 20mL up to control medicinal material solution.
Take medicinal material the kuh-seng 7.5g, frutus cnidii 7.5g, polygonum cuspidate 7.5g crushed in advance through FW type electric crusher, climbing groundsel 7.5g, smilax 7.5g, paniculate swallowwort 7.5g, Radix Glycyrrhizae 5g, folium panacis japonici cum caule 5g, radix paeoniae rubra 4g, Chinese prickly ash 2.5g, menthol 0.05g fine powder are put It is placed in 500mL conical flask, proper amount of methanol (submergence medicinal material) is added, ultrasound is stood in KQ-100DB type numerical control ultrasonic cleaning machine 25min, filtering, gained filtrate is negative control sample.
It contains 5~10mL ammonium hydroxide with small beaker first to be placed in chromatography cylinder, while will be by the silica gel g thin-layer plate of non-point sample It is placed in cylinder, covers glass plate saturation presaturation 15min.Then test solution, comparison medicine are drawn respectively with point sample capillary Material solution, negative control sample solution is appropriate, point on the silica G plate of saturation, with now match n-butanol-glacial acetic acid-water (7: 2: 1) solution 20mL is solvent, stands expansion in exhibition cylinder, then takes out to be placed in draught cupboard and dry, ultraviolet in WD-9403A It is inspected in instrument with 365nm ultraviolet lamp.As a result the spot of test sample and control medicinal material sample in corresponding position all displaing yellows.Such as Shown in Fig. 2~5.
2.4.2 the thin layer of radix paeoniae rubra identifies
It takes sample solution 10mL in ceramic whiteware ware with pipette, is placed on 80 DEG C of HH digital display thermostat water baths and steams to close Dry, residue obtained plus proper amount of methanol is allowed to dissolve, be subsequently placed in ultrasonic treatment 5 in KQ-100DB type numerical control ultrasonic cleaner~ 10min then takes out and filters solution, obtains sample solution.
Paeoniflorin reference substance solution is provided by Huaihua food and medicine inspection institute
Take fine medicinal material powder kuh-seng 7.5g, frutus cnidii 7.5g, polygonum cuspidate 7.5g, smilax 7.5g, climbing groundsel 7.5g, Cortex Phellodendri 7.5g, paniculate swallowwort 7.5g, folium panacis japonici cum caule 5g, Radix Glycyrrhizae 5g, Chinese prickly ash 2.5g, menthol 0.05g are added appropriate in 500mL conical flask Methanol (submergence medicinal material) ultrasound 25min.Filtering, gained filtrate is negative controls solution.
With point sample capillary pipette samples solution, reference substance solution, negative controls solution is appropriate, is put respectively in same silicon It is solvent in exhibition cylinder exhibition with the chloroform now matched-ethyl acetate-methyl alcohol-formic acid (40: 5: 10: 0.2) solution on glue G lamellae It opens, takes out, lay flat and dry in draught cupboard, spray with 5% vanillin-sulfuric acid solution, dried in electric drying oven with forced convection, to aobvious Color taking-up is set in ultraviolet justice and is inspected with fluorescent lamp.Sample and reference substance chromatography are in the aobvious bluish violet spot in corresponding position.As Fig. 6~ Shown in 9.
2.4.3 the thin layer of polygonum cuspidate identifies
It measures sample 10mL, in sulfuric acid 1mL and round-bottomed flask, fills water with 500mL beaker and do water-bath in heating in heating mantle, Flask is set and is heated to reflux 30min in being heated to reflux device in water-bath, is taken out after cooling, with chloroform extraction 2 times, every time 20mL finally merges chloroform liquid in evaporating dish, sets and be evaporated in water-bath, and residue adds 2mL methanol to be allowed to dissolution to get test sample Solution.
Rheum emodin reference substance (offer of Huaihua medicine inspecting institute)
Weigh medicinal material kuh-seng 7.5g, Cortex Phellodendri 7.5g, smilax 7.5g climbing groundsel 7.5g, radix paeoniae rubra 7.5g, paniculate swallowwort 7.5g, people Join leaf 5g, Radix Glycyrrhizae 5g, frutus cnidii 7.5g, Chinese prickly ash 2.5g, menthol 0.05g fine powder is set in 500mL conical flask, appropriate first is added Alcohol (submergence medicinal material), ultrasonic extraction 25min.Then by the medical filtration after ultrasonic extraction, gained filtrate is negative control sample Liquid.
Appropriate with the above-mentioned 3 kinds of solution of point sample capillary absorption, point sample is in silica G plate respectively, with the n-hexane-acetic acid now matched Ethyl ester-formic acid (6:2:0.1) solution 10mL is that solvent is unfolded in exhibition cylinder, takes out, sets in draught cupboard and dry, set under fluorescent lamp It inspects.Sample chromatogram and reference medicine chromatography on a corresponding position, all show the spot of phase yellow.As shown in Figure 10~13.
2.4.4 the thin layer of menthol identifies
Sample 30mL is measured, adds diethyl ether and is extracted 2 times, each 30mL in separatory funnel, aqueous leaves and takes subsequent spare, merging Ether solution.Suitable anhydrous sodium sulfate is added to be dehydrated, filtration, filtrate volatilizes residue obtained plus ethyl alcohol 1ml dissolution, and as test sample is molten Liquid [11].
Menthol reference substance 10mg is taken, ethyl alcohol 5mL is added to dissolve, obtaining content is 2mg/mL reference substance solution.
Weigh fine medicinal material powder Cortex Phellodendri 7.5g, kuh-seng 7.5g, frutus cnidii 7.5g, climbing groundsel 7.5g, paniculate swallowwort 7.5g, polygonum cuspidate 7.5g, radix paeoniae rubra 7.5g, folium panacis japonici cum caule 5g, Radix Glycyrrhizae 5g, smilax 7.5g, Chinese prickly ash 2.5g are added in 500mL conical flask and do not cross medicinal material Conical flask is placed in ultrasonic device ultrasonic soak extraction 25min by the methanol of amount.Then extracting solution is filtered, filtrate is negative right According to solution.
It takes point sample capillary to be drawn on a small amount of respectively and prepares solution, at interval of 1~1.5cm point one on same silica G plate Sample spot pipettes solvent 15mL cyclohexane-ethyl acetate (17:3) solution of existing preparation in exhibition layer cylinder, silica gel plate is placed in Expansion is stood in developing agent, is taken out, is placed in draught cupboard and dries, and is sprayed with 5% vanillin-sulfuric acid solution, in electric heating forced air drying It is clear that in 105 DEG C spot development is heated in case.It takes out, inspection is known under fluorescent light.As a result test sample and reference substance are in corresponding positions Set the spot for all showing blue.As shown in Figure 14~17.
2.4.5 the thin layer of folium panacis japonici cum caule identifies
It takes menthol thin layer to identify aqueous spare under test sample preparation, water saturated butanol solution is then added 20ml shaking washing (washing 2 times) merges n-butanol extracting liquid twice, then washs extracting solution with ammonia solution 20mL again, discard ammonia Solution.Water washing 2 times be saturated again with n-butanol, each 20mL finally discards aqueous, by combined butanol solution in water-bath Upper heating concentration, final residuum 2mL methanol dissolve, and obtain test sample solution.
Reference substance ginsenoside Rb1, ginsenoside Re, ginsenoside Rg1 (by Huaihua, medicine inspecting institute is provided).
Weigh radix paeoniae rubra 7.5g, Cortex Phellodendri 7.5g, kuh-seng 7.5g, smilax 7.5g climbing groundsel 7.5g, frutus cnidii 7.5g, polygonum cuspidate 7.5g, paniculate swallowwort 7.5g, Radix Glycyrrhizae 4g, Chinese prickly ash 2.5g, menthol 0.05g fine medicinal material powder are set in 500mL beaker, and it is suitable that methanol is added Amount (submergence medicinal material), the ultrasound 25min in ultrasonic cleaner.Extracting solution takes out filtering, and filtrate is negative control sample.
It is appropriate that above-mentioned sample solution is drawn respectively with 0.3mm point sample capillary, is put on same silica gel g thin-layer plate, is taken just Butanol-ethyl acetate-water (4:1:5) mixed liquor upper layer 20mL is solvent, is placed in chromatography cylinder, while in another slot of cylinder It measures into 1mL sulfuric acid solution.Expansion is stood, is taken out, is placed in draft chamber and dries, is sprayed with 10% ethanol solution of sulfuric acid, at 80 DEG C It is clear that it is heated to spot development in DHG9145A electric heating constant-temperature blowing drying box, is inspected under daylight.As a result test sample and reference substance Chromatography on a corresponding position, shows the spot of same color.As shown in Figure 18~21.
2.4.6 the thin layer of Radix Glycyrrhizae identifies
Sample 30mL is pipetted with pipette, is transferred in separatory funnel, the good water saturated n-butanol of configured in advance is added 20mL shaking out washes twice, merges n-butanol extracting liquid, then washs extraction merging liquid with the water 20mL that n-butanol is saturated, It is equally extracted twice, discards aqueous, extraction solution is placed in heating water bath in evaporating dish and is concentrated to dryness, it is cooling, then plus 1mL first Alcohol dissolution mixes to get test solution.
Control medicinal material solution: weighing Radix Glycyrrhizae fine powder 1.5g in a round bottom flask, adds 100mL water, connects reflux unit, reflux 30min is decocted, takes out and stands cooling, then filter, heating water bath is concentrated into 50mL to gained filtrate again.Concentration decoction liquor is added into water The n-butanol 20mL of saturation is extracted 2 times, merges upper layer extracting solution twice, then plus 20mL n-butanol saturation water washing, discard down Layer aqueous.The heating of above-mentioned butanol extraction liquid is concentrated to dryness, dissolved when adding 1mL methanol to get.
Medicinal material frutus cnidii 7.5g, Cortex Phellodendri 7.5g are weighed, kuh-seng 7.5g, smilax 7.5g climbing groundsel 7.5g, polygonum cuspidate 7.5g are taken, Radix paeoniae rubra 7.5g, paniculate swallowwort 7.5g, folium panacis japonici cum caule 5g, Chinese prickly ash 2.5g, menthol 0.05g fine powder are set in 500mL beaker, are added appropriate Methanol (submergence medicinal material), ultrasonic 25min.Filtering, filtrate is negative control sample.
It is appropriate that above-mentioned three kinds of solution is drawn respectively with 0.3mm point sample capillary, and point is matched in advance in taking on same silica G plate The acetic ether-methanoic acid of system-glacial acetic acid-water (15:1:1:2) 20mL is solvent, and expansion, taking-up, which is placed in draft chamber, dries, 10% ethanol solution of sulfuric acid is sprayed, colour developing is heated in 105 DEG C of electric drying oven with forced convections, is inspected under ultraviolet lamp fluorescent lamp.As a result it supplies Test product and control medicinal material on a corresponding position, show the spot of same color.As shown in Figure 22~25.
The quantitative identification of 2.5 technique finished products
2.5.1 chromatographic condition
Shim-pach GISS C18 (2.1mm × 100mm, 1.9 μm) chromatographic column, octadecylsilane chemically bonded silica filling Agent, mobile phase are acetonitrile -0.05mol/L potassium dihydrogen phosphate (phosphoric acid tune PH to 4) system, flow velocity: 0.15mLminˉ1, column Temperature: 30 DEG C, Detection wavelength is respectively matrine 220nm, Berberine hydrochloride 365nm, and sample volume is 10 μ L.Chromatographic condition is gradient Elution.
2.5.2 the preparation of reference substance solution
Precision weighing matrine reference substance 10mg adds methanol dissolution to mix to scale, shakes up in 10mL volumetric flask.Obtain concentration For the matrine reference substance stock solution of 1.0mg/mL.
Precision weighing 0.5mg jamaicin reference substance, is transferred in 10mL volumetric flask, methanol dilution to scale is added to shake up.System It is reference substance stock solution at the Berberine hydrochloride that concentration is 0.05mg/mL.
Hybrid standard reference substance solution (Berberine hydrochloride: 0.005mg/mL, matrine: 0.6mg/mL): from 0.05mg/mL It measures 0.5mL in Berberine hydrochloride reference substance solution to set in 5mL volumetric flask, then accurate measurement matrine reference substance stock solution 3mL It sets in same volumetric flask, adds methanol to scale, mix.
2.5.3 the preparation of test sample solution
Precision pipettes 5mL process sample liquid in separatory funnel, adds ammonium hydroxide 2mL shaking to mix alkalization, is extracted with methylene chloride Take washing 3 times, each 20mL.Merge lower layer's extracting solution (methylene chloride density ratio water is big), is transferred in evaporating dish in 60 DEG C of water It is evaporated in bath, it is cooling, add methanol to dissolve washing evaporating dish (repeatedly washing, every time on a small quantity, until solution transfer is complete), cleaning solution turns It moves on in 10mL volumetric flask, is then added dropwise again and adds the dilute polishing scale of methanol, shake up.Then one times is diluted, therefrom accurate amount 5mL solution is added dropwise methanol to scale, shakes up into another clean spare 10mL volumetric flask.
2.5.4 assay result
The content (n=3) of 3.2 matrine of table and Berberine hydrochloride
In the experiment of this technical study, by obtained by membrane filtration, centrifugation three kinds of different process of membrane filtration and alcohol precipitation Sample carry out product yield, solid content, clarity, thin layer identify and the measurement of evaluation indexes such as matrine content with it is right Than come the feasibility of studying membrane filtration processes.In an experiment, before concentrate is without process, solid content is 18.05%, the content of matrine and jamaicin is respectively 1.28mg/ml and 0.063mg/ml.Only carry out the sample B of membrane filtration processes Product yield is 97%, solid content 13.50%；The sample C product yield of membrane filtration processes is 95% again after being centrifuged, Gu Shape object content is 10.09%；It is 88% through sample D product yield obtained by alcohol precipitation process, solid content 19.52%, thus It can be seen that the process sample solid content after being centrifuged membrane filtration is obviously less.And by the testing result of clarity it is found that institute Sample is obtained without visible foreign matters, is complied with standard.By to three's sample Qualitive test, can obtain three kinds of techniques to medical fluid mainly at Point character all has no significant effect.By the quantitative identification experiment of three of the above technique finished product, (B sample matrine content is 1.30mg/ Ml, content of berberine 0.069mg/ml；C sample matrine content is 1.62mg/ml, content of berberine 0.075mg/ml, D Sample matrine content can be seen that for 1.54mg/ml, content of berberine 0.082mg/ml) result, after being centrifuged membrane filtration processes Finished product matrine and the comprehensive content of jamaicin are higher.Show to be centrifuged in conclusion being compared the quality index result of three Membrane filtration processes can be reduced solid content afterwards, small to main component affect trait, and product yield liquid is higher.
Take test sample sample A (concentrate) respectively, sample B (medical fluid after membrane filtration), sample the C (medicine of membrane filtration after centrifugation Liquid), each six parts of 50ml of sample D (supernatant after alcohol precipitation) is packed into the polyester bottles of liquid, medicinal.In 40 DEG C ± 2 DEG C of temperature, relatively wet It is placed 3 months under conditions of degree 75% ± 5%.2 bottles of detections are taken every time.The stable type of sample is investigated by accelerated stability test. Test item includes character, relative density, pH value, identification, content, and test result is as shown in table 3.3~3.7.
3.3 washing lotion character of table compares
The pH value of 3.4 washing lotion of table compares
The relative density of 3.5 washing lotion of table changes
3.6 determination of matrine result (mg/mL) of table
3.7 berberine hydrochloride content result (mg/mL) of table
The above results show that sample obtained by membrane filtration processes is good compared with other technology stabilities after the centrifugation of the application.
The embodiments described above only express several embodiments of the present invention, and the description thereof is more specific and detailed, but simultaneously Limitations on the scope of the patent of the present invention therefore cannot be interpreted as.It should be pointed out that for those of ordinary skill in the art For, without departing from the inventive concept of the premise, various modifications and improvements can be made, these belong to guarantor of the invention Protect range.Therefore, the scope of protection of the patent of the invention shall be subject to the appended claims.

Claims (3)

1. a kind of impurity-removing method of clean negative itching-relieving lotion, which comprises the following steps:
After clean negative itching-relieving lotion centrifugation, after filtering with microporous membrane, filtrate is completed into removal of impurities using ultrafiltration membrance filter.
2. the impurity-removing method of clean negative itching-relieving lotion according to claim 1, which is characterized in that the centrifugal condition is centrifugation Revolving speed is 1500~3000 turns/min, and when centrifugation is 15~30 minutes a length of.
3. the impurity-removing method of clean negative itching-relieving lotion according to claim 1 or 2, which is characterized in that the miillpore filter Aperture is 0.45-0.22 microns, and it is 0.05-0.15MPa, flow velocity 0.1-0.5m/s, the hole of the ultrafiltration membrane that filtering, which applies pressure, Diameter is 2-50 nanometers, and it is 0.01-0.1MPa, flow velocity 0.1-0.5m/s that filtering, which applies pressure,.
CN201811369191.3A 2018-11-16 2018-11-16 The impurity-removing method of clean yin itching-relieving lotion Pending CN109550006A (en)

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Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101215422A (en) * 2008-01-21 2008-07-09 中国林业科学研究院资源昆虫研究所 Method for refining lac red coloring matter
CN103520284A (en) * 2013-09-27 2014-01-22 河南牧翔动物药业有限公司 Method for preparing veterinary Shuanghuanglian oral liquid through enzyme assistance
CN105267269A (en) * 2015-10-27 2016-01-27 天津市红特顺科技有限公司 Method using membrane technology to separate effective constituents in medicinal materials

Patent Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101215422A (en) * 2008-01-21 2008-07-09 中国林业科学研究院资源昆虫研究所 Method for refining lac red coloring matter
CN103520284A (en) * 2013-09-27 2014-01-22 河南牧翔动物药业有限公司 Method for preparing veterinary Shuanghuanglian oral liquid through enzyme assistance
CN105267269A (en) * 2015-10-27 2016-01-27 天津市红特顺科技有限公司 Method using membrane technology to separate effective constituents in medicinal materials

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