CN106074749A - A kind of pollen is dispelled pain-easing spray and preparation method thereof of itching - Google Patents

A kind of pollen is dispelled pain-easing spray and preparation method thereof of itching Download PDF

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CN106074749A
CN106074749A CN201610479159.5A CN201610479159A CN106074749A CN 106074749 A CN106074749 A CN 106074749A CN 201610479159 A CN201610479159 A CN 201610479159A CN 106074749 A CN106074749 A CN 106074749A
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ethanol
add
vinegar
parts
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龙凤荣
李珂
王瑶
孙敏
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GUIZHOU HONGKANG PHARMACEUTICAL CO Ltd
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GUIZHOU HONGKANG PHARMACEUTICAL CO Ltd
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    • A61K36/18Magnoliophyta (angiosperms)
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    • A61K36/71Ranunculaceae (Buttercup family), e.g. larkspur, hepatica, hydrastis, columbine or goldenseal
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Abstract

The invention discloses a kind of pollen to dispel pain-easing spray and preparation method thereof of itching, this spray is mainly fabricated to external spraying agent by Radix Trichosanthis, the Radix Angelicae Dahuricae, Radix Aconiti Brachypodi (Radix Aconiti Szechenyiani), Borneolum Syntheticum, Camphora, Olibanum (processed with vinegar), Myrrha (processed with vinegar), Oleum menthae, Oleum Eucalypti and adjuvant.The present invention is according to the character of medicine each in pollen itching-dispelling pain-relieving tincture prescription, and the effect that this medicine is played in prescription, is made into spray, and substrate used is screened, substrates quantity is optimized so that drug effect dramatically increases, is suitable for all kinds of patients and uses., being improved concrete processing technology and parameter, substrate and processing technology of the present invention combine, and promote the dissolution effectively becoming 11 carbonyls β acetyl boswellic acid (AKBA) in Olibanum in the dissolution of effective ingredient, especially Olibanum meanwhile.Making the more refine of this medicine, drug effect is more significantly, and clinical efficacy is good.

Description

A kind of pollen is dispelled pain-easing spray and preparation method thereof of itching
Technical field
The present invention relates to a kind of pollen dispel pain-easing spray and preparation method thereof of itching, belong to the field of medicine technology.
Technical background
Traumatic injury is in daily life for some people seemingly homely food, and Chinese traditional treatment traumatic injury has thousand of The history in year, ancient " traumatic injury " is called the introduction of all wounds, how because of External Force Acting, or in the case of self fault firmly Too quickly and cause.Muscles and bones trauma that the traditional Chinese medical science causes in human body because of External Force Acting all, swelling and pain due to blood stasis, disharmony between QI and blood, meridians Obstructed so that internal organs are impaired etc., it is referred to as traumatic injury.Its main pathology is that congestion is stopped up stagnant, and blood is held one's breath resistance, therefore with pain, swelling For main performance.Treatment is many with promoting blood circulation to remove obstruction in the collateral, relaxing muscles and tendons and promoting circulation of QI, and reducing swelling and alleviating pain is method, and curative effect is the most obvious.
Pollen itching-dispelling pain-relieving tincture comes from ethnic groups medication among the people, and Radix Aconiti Brachypodi (Radix Aconiti Szechenyiani) has strong analgesic activity, for principal agent, Be aided with the Radix Angelicae Dahuricae, Radix Trichosanthis is ministerial drug, has detumescence, antipruritic effect, helps Radix Aconiti Brachypodi (Radix Aconiti Szechenyiani) to play antiinflammatory, analgesic efficacy;Pain is then Obstructed, the most bitterly, Gu Zuo is to have the Olibanum of blood circulation promoting and blood stasis dispelling, promoting the circulation of QI to relieve pain, Myrrha for general rule.We have blood circulation promoting and blood stasis dispelling, and detumescence is only Bitterly, effect of dispelling wind for relieving itching, we are for blood circulation promoting and blood stasis dispelling, and reducing swelling and alleviating pain, dispelling wind for relieving itching, effect is obvious.But owing to tincture containing Having substantial amounts of ethanol, the patient of alcohol sensible should not be suitable for by skin, and tincture ethanol during storing is readily volatilized, can shadow Ring the curative effect of medicine.Additionally, applicant further found that, use existing extraction process to make pollen and dispel and itch in analgetic preparation, Olibanum Effective ingredient is difficult to measure, and the content of especially 11-carbonyl-beta-acetyl boswellic acid is difficult to measure.Pollen is dispelled pain relieving system of itching The clinical efficacy of agent is the most preferable.
Medicinal herb spray, is to be mixed with suitable additives by Chinese medicine extract or fine medicinal material powder.Chinese medical spray Agent effect is rapid, can can form thin film in surface with dosed administration, favorably play drug effect as tcm emergency medication, Curative effect is fast.
As pollen itching-dispelling pain-relieving tincture is made spray, will be enlarged by its scope of application, be preferably patient service.
Summary of the invention:
It is an object of the invention to, it is provided that a kind of pollen is dispelled pain-easing spray and preparation method thereof of itching.The present invention is according to flower Powder is dispelled the character of each medicine in analgesic tincture prescription of itching, and the effect that this medicine is played in prescription, is made into spray, and Substrate used is screened, substrates quantity is optimized so that drug effect is dramatically increased, be suitable for all kinds of patients and use. , being improved concrete processing technology and parameter, substrate of the present invention and processing technology of the present invention combine, and promote Olibanum meanwhile The dissolution of middle effective ingredient, especially Olibanum effectively become the dissolution of 11-carbonyl-beta-acetyl boswellic acid (AKBA).Make this medicine Thing more refine, drug effect is more significantly, and clinical efficacy is good.
For solving above-mentioned technical problem, the present invention realizes by the following technical solutions: a kind of pollen is dispelled pain-easing spray of itching, By Radix Trichosanthis 30-60 part in parts by weight, Radix Angelicae Dahuricae 30-60 part, Radix Aconiti Brachypodi (Radix Aconiti Szechenyiani) 20-50 part, Borneolum Syntheticum 1-8 part, Camphora 1-8 Part, Olibanum (processed with vinegar) 10-30 part, Myrrha (processed with vinegar) 10-30 part, and by volume Oleum menthae 5-30 part of part meter, Oleum Eucalypti 1-8 part, glycerol 30-40 part, and the sodium sulfite 0.1-0.8 part calculated by weight, disodiumedetate 0.1-0.8 part and distillation Water 30-50 part is made.
Aforesaid pollen is dispelled pain-easing spray of itching, and by Radix Trichosanthis 45 parts in parts by weight, the Radix Angelicae Dahuricae 45 parts, avenges one Artemisia 34 parts, Borneolum Syntheticum 4 parts, Camphora 5 parts, Olibanum (processed with vinegar) 20 parts, Myrrha (processed with vinegar) 20 parts, and the by volume Oleum menthae 10 parts of part meter, eucalyptus globulus Oil 5 parts, glycerol 35 parts, and the sodium sulfite calculated by weight 0.4 part, disodiumedetate 0.4 part and distillation 40 parts of water is made.
A kind of aforesaid pollen is dispelled the manufacture method of pain-easing spray of itching, and comprises the following steps:
(1) taking Radix Trichosanthis, Radix Aconiti Brachypodi (Radix Aconiti Szechenyiani), Myrrha (processed with vinegar), the Radix Angelicae Dahuricae is ground into coarse granule, mixing, adds the leaching of 75-85% ethanol Moisten 20-28 hour, then impregnate in three times with 75-85% ethanol, for the first time during 2-4;Second and third time each 1-3 hour, merges 3 times Impregnation liquid, filters, must mix filtrate standby, standby;Take Olibanum again, use water vapour distillation volatile oil, standby;Medicinal residues add again Enter the ethanol solution of 3-5 times amount 75-85%, reflux, extract, 1-3 time, each 0.5-1.5h, filter, merging filtrate, reclaim ethanol To only, obtain alcohol extract, alcohol extract and mixing filtrate and merge, obtain A product;
(2) separately take Borneolum Syntheticum, Camphora, Oleum menthae, Oleum Eucalypti add 75-85% ethanol and dissolve, and add in A product, then add 75-85% second Alcohol makes into 900-1100ml, mixing, stands 20-28 hour, takes supernatant, filters, obtains B product;
(3) take sodium sulfite and disodiumedetate is dissolved in distilled water, after dissolving, obtain C product;
(4) in C product, add B product, glycerol and above-mentioned volatile oil, stir evenly, place, filter, subpackage, to obtain final product.
Aforesaid pollen is dispelled the manufacture method of pain-easing spray of itching, and comprises the following steps:
(1) taking Radix Trichosanthis, Radix Aconiti Brachypodi (Radix Aconiti Szechenyiani), Myrrha (processed with vinegar), the Radix Angelicae Dahuricae is ground into coarse granule, mixing, adds 80% ethanol infiltration 24 hours, then impregnate in three times with 80% ethanol, 3 hours for the first time;Second and third time each 2 hours, merges 3 impregnation liquid, filter Cross, filtrate must be mixed, standby;Take Olibanum (processed with vinegar) again, use water vapour distillation volatile oil, standby;Medicinal residues add 4 times amount The ethanol solution of 80%, reflux, extract, 2 times, each 1h, filter, merging filtrate, recovery ethanol, to only, obtains alcohol extract, alcohol extraction Take liquid and mixing filtrate merges, obtain A product;
(2) separately take Borneolum Syntheticum, Camphora, Oleum menthae, Oleum Eucalypti add 80% ethanol and dissolve, and add in A product, then add 80% ethanol and make into 1000ml, mixing, stand 24 hours, take supernatant, filter, obtain B product;
(3) take sodium sulfite and disodiumedetate is dissolved in distilled water, after dissolving, obtain C product;
(4) in C product, add B product, glycerol and above-mentioned volatile oil, stir evenly, place, filter, subpackage, to obtain final product.
In drug prescription of the present invention, Radix Aconiti Brachypodi (Radix Aconiti Szechenyiani) has strong analgesic activity, for principal agent, is aided with the Radix Angelicae Dahuricae, variola Powder is ministerial drug, has detumescence, antipruritic effect, helps antiinflammatory, analgesic efficacy that Radix Aconiti Brachypodi (Radix Aconiti Szechenyiani) plays, and pain is the most obstructed, and general rule is not Bitterly, Gu Zuo is to have the Olibanum of blood circulation promoting and blood stasis dispelling, promoting the circulation of QI to relieve pain, Myrrha.There is blood circulation promoting and blood stasis dispelling, reducing swelling and alleviating pain, the merit of dispelling wind for relieving itching Effect.Applicant has carried out long numerous studies to pollen analgetic preparation, and applicant with Radix Trichosanthis, the Radix Angelicae Dahuricae, avenges upper one at first Branch Artemisia, Borneolum Syntheticum, Camphora, Olibanum (processed with vinegar), Myrrha (processed with vinegar), Oleum menthae and Oleum Eucalypti are that tincture made by raw material, but because tincture is containing substantial amounts of Ethanol, the patient of alcohol sensible should not be suitable for by skin, and tincture ethanol during storing is readily volatilized, can affect medicine Curative effect.Again because spray is as carrier transdermal administration, having unique advantage compared with other dosage forms, medicinal herb spray effect is fast Speed, can can form thin film with dosed administration, favorably play drug effect as tcm emergency medication in surface, and curative effect is fast.
Therefore, applicant considers to be made into spray, but after being formed into spray, substrate accounts for the biggest portion of spray Point, the quality of spray is played an important role.Good for guaranteeing spray quality of the present invention, drug effect is good, and applicant is to spray The selection of substrate and consumption carried out substantial amounts of research, applicant draws through lot of experiments, selects ethyl cellulose, poly- When vinylpyrrolidone K-30, olefin(e) acid resin, tween 1 and corn protein are substrate.The pollen made is dispelled pain-easing spray of itching Drug effect is preferable.And curative effect is better than the curative effect of former tincture.
Additionally, existing pollen is also dispelled by applicant, the itch processing technology of analgetic preparation is improved, and existing pollen is dispelled and itched The manufacture method method of analgetic preparation is: Radix Trichosanthis, the Radix Angelicae Dahuricae, Radix Aconiti Brachypodi (Radix Aconiti Szechenyiani), Olibanum (processed with vinegar), Myrrha (processed with vinegar) are ground into thick Grain, mixing, add 80% ethanol infiltration 24h, then impregnate in three times with 80% ethanol, 3 hours for the first time, second and third each 2h, close And 3 impregnation liquid, filtering, filtrate is standby;Separately take Borneolum Syntheticum, Camphora, Oleum menthae, Oleum Eucalypti add 80% ethanol and dissolve, and add above-mentioned filter In liquid, then add 80% ethanol and make into 1000ml, mixing, stand 24h, take supernatant, filter, to obtain final product.But inventor is in research During find, adopting the pollen made in this way and dispel and itch in analgetic preparation, the effective ingredient of Olibanum is difficult to measure.Make breast Fragrant clinical efficacy is the most preferable.Inventor also finds in technical study, uses the inventive method individually to be extracted by Olibanum And changing the extraction process of Olibanum, the pollen so made is dispelled and is itched in analgetic preparation, and the effective ingredient of Olibanum is easily measured, and surveys The effective ingredient of the Olibanum gone out is high.This allows for so that the more refine of this medicine, and drug effect is more significantly, and clinical efficacy is good.Application People also finds, uses present invention process and coordinates above-mentioned substrate, can better promote the dissolution of effective ingredient in Olibanum, especially It is the dissolution of 11-carbonyl-beta-acetyl boswellic acid, promotees the effect of oozing and become apparent from, the 11-carbonyl itched in analgetic preparation so that pollen is dispelled Base-β-acetyl boswellic acid (AKBA) improves, and the boswellic acids (BAs) in Olibanum is the effective of effect such as its antiinflammatory, antitumor etc. Composition, wherein 11-carbonyl-beta-acetyl boswellic acid (AKBA) anti-inflammatory activity is the most notable, therefore, 11-carbonyl-beta-acetyl boswellic acid (AKBA), after dissolution improves, drug effect is more preferable, so that its clinical effectiveness is more preferable.
Compared with prior art, the present invention is according to the character of medicine each in pollen itching-dispelling pain-relieving tincture prescription, and this medicine Effect played in prescription, is made into spray, and is screened substrate used, carried out excellent to substrates quantity Change so that drug effect dramatically increases, be suitable for all kinds of patients and use.Meanwhile, concrete processing technology and parameter are improved, substrate Combine with processing technology of the present invention, promote in Olibanum the dissolution of effective ingredient, especially Olibanum effectively become 11-carbonyl-β- The dissolution of acetyl boswellic acid (AKBA).Making the more refine of this medicine, drug effect is more significantly, and clinical efficacy is good.
Applicant carried out following experiments, the provable present invention has effective effect;
Experimental example 1: pharmacodynamic study
Applicant has carried out Pharmacodynamics research to the present invention, by experimental data, beneficial effects of the present invention is described.
1, analgesic test
1.1 Experimental agents
Spray the most of the present invention: make by embodiment 1;
1.1.2 former tincture:
Prescription: Radix Trichosanthis 45g, Radix Angelicae Dahuricae 45g, Radix Aconiti Brachypodi (Radix Aconiti Szechenyiani) 34g, Borneolum Syntheticum 4g, Camphora 5g, Olibanum (vinegar system) 20g, Myrrha (vinegar system) 20g, Oleum menthae 10ml, Oleum Eucalypti 5ml;
Technique: first take Radix Trichosanthis, the Radix Angelicae Dahuricae, Radix Aconiti Brachypodi (Radix Aconiti Szechenyiani), Olibanum, Myrrha pulverizing, mixing, adds 80% ethanol infiltration 24h, Impregnating in three times with 80% ethanol, 3h for the first time, second and third each 2h again, merge 3 impregnation liquid, filter, filtrate is standby;Separately Take Borneolum Syntheticum, Camphora, Oleum menthae, Oleum Eucalypti add 80% ethanol and dissolve, and add in above-mentioned filtrate, then add 80% ethanol and make into 1000ml, Mixing, stands 24h, takes supernatant, filters, makes tincture.
1.2 experimental technique
Take healthy Kunming mouse 48, male and female half and half, be randomly divided into 3 groups, i.e. blank group, spray group of the present invention (making according to the method for the embodiment of the present invention 1) and former tincture group, often group 16.Dosage is respectively blank group (0.5g/kg excipient), of the present invention group (0.5g/kg spray of the present invention group), former tincture group (0.5g/kg).Mice buttocks is carried on the back Losing hair or feathers in portion, gives corresponding tested material, give 2h, be administered once daily, successive administration 3 days.In last after medicine 12h, each mice Only, in observed and recorded 15min, there is the number of times of writhing response, meter to lumbar injection 0.8% white vinegar acid solution 0.2ml/ in every mice Calculate mean and standard deviation, compare group difference.
1.3 result
Each administration group all can resist the pain reaction caused by white vinegar acid stimulation, makes mouse writhing number of times significantly reduce and (is shown in Table 1)。
The table 1 impact (n=12, x ± s) on mouse writhing number of times
Note: spray group of the present invention compares with former tincture group*P < 0.05;
Compare with blank group##P < 0.01
1.4 conclusion
Above experimental studies results shows, spray group of the present invention and former tincture group all can be resisted caused by white vinegar acid stimulation Pain reaction (P < 0.01), but spray group of the present invention is better than former tincture group (P < 0.05).
2, antiinflammatory experiment
2.1 Experimental agents
Spray the most of the present invention: make by embodiment 1;
2.2.2 former tincture:
Prescription: Radix Trichosanthis 45g, Radix Angelicae Dahuricae 45g, Radix Aconiti Brachypodi (Radix Aconiti Szechenyiani) 34g, Borneolum Syntheticum 4g, Camphora 5g, Olibanum (vinegar system) 20g, Myrrha (vinegar system) 20g, Oleum menthae 10ml, Oleum Eucalypti 5ml;
Technique: first take Radix Trichosanthis, the Radix Angelicae Dahuricae, Radix Aconiti Brachypodi (Radix Aconiti Szechenyiani), Olibanum, Myrrha pulverizing, mixing, adds 80% ethanol infiltration 24h, Impregnating in three times with 80% ethanol, 3h for the first time, second and third each 2h again, merge 3 impregnation liquid, filter, filtrate is standby;Separately Take Borneolum Syntheticum, Camphora, Oleum menthae, Oleum Eucalypti add 80% ethanol and dissolve, and add in above-mentioned filtrate, then add 80% ethanol and make into 1000ml, Mixing, stands 24h, takes supernatant, filters, makes tincture.
2.2 experimental technique
2.2.1 mice ear experiment takes healthy Kunming mouse 48, male and female half and half, and packet, dosage are with 1.1 Under, successive administration 6 days, within the 7th day, give 20 μ L dimethylbenzene by every mouse right ear one side, another side gives 10 μ L.Locate after 30min Dead animal, beats with 8mm card punch and takes left and right ear same position disk, weigh, and calculates swelling rate=(auris dextra weight-left ear weight Amount)/left ear weight × 100%.The results are shown in Table 2.
2.2.2 rat paw edema experiment takes male Kunming kind rat 48, is randomly divided into 3 groups, and packet is with 2.2.1 item Under.Rat abdomen depilation area is 2.5cm × 2.5cm.Spray group external application 0.3g/kg of the present invention, gives outside former tincture group 0.3g/kg, blank group external application bare substrate 0.3g/kg, give 2h, every day 1 time, successive administration 6 days.Survey big with volumetric method Normal foot sole of the foot volume (mL) of the right metapedes of Mus.After last is administered, Rat Right metapedes plantar subcutaneous injection 1% carrageenin 0.1mL causes Inflammation, the sufficient sole of the foot volume of 5h same position after survey cause inflammation.Calculating swelling rate=(causing the scorching front foot sole of the foot thickness of scorching metapedes sole of the foot thickness-cause)/ Cause scorching front foot sole of the foot thickness × 100%.The results are shown in Table 3.
Table 2 mice is turned round auricle edema rate and compares (n=12, x ± s)
Note: compare with former tincture group*P < 0.05;
Compare with blank group#P < 0.05,##P < 0.01.
Table 3 is respectively organized rat paw edema rate and is compared (n=12, x ± s)
Note: compare with former tincture group*P < 0.05;
Compare with blank group#P < 0.05,##P < 0.01.
2.3 conclusion
Result shows: spray group of the present invention and former tincture group all can reduce mice and turn round auricle edema rate and rat paw edema Rate.Comparing with former tincture group, spray group effect of the present invention is more preferably (P < 0.05).
3, dispel test of itching
3.1 Experimental agents
Spray the most of the present invention: (making by embodiment 1);
3.2.2 former tincture:
Prescription: Radix Trichosanthis 45g, Radix Angelicae Dahuricae 45g, Radix Aconiti Brachypodi (Radix Aconiti Szechenyiani) 34g, Borneolum Syntheticum 4g, Camphora 5g, Olibanum (vinegar system) 20g, Myrrha (vinegar system) 20g, Oleum menthae 10ml, Oleum Eucalypti 5ml;
Technique: first take Radix Trichosanthis, the Radix Angelicae Dahuricae, Radix Aconiti Brachypodi (Radix Aconiti Szechenyiani), Olibanum, Myrrha pulverizing, mixing, adds 80% ethanol infiltration 24h, Impregnating in three times with 80% ethanol, 3h for the first time, second and third each 2h again, merge 3 impregnation liquid, filter, filtrate is standby;Separately Take Borneolum Syntheticum, Camphora, Oleum menthae, Oleum Eucalypti add 80% ethanol and dissolve, and add in above-mentioned filtrate, then add 80% ethanol and make into 1000ml, Mixing, stands 24h, takes supernatant, filters, makes tincture.
3.2 experimental technique
Take Cavia porcellus 50, be divided into blank group (bare substrate), spray group of the present invention at random;Former tincture group.Respectively Dorsal portion shaving 1.5cm × 1.5cm behind the group Cavia porcellus right side, is uniformly applied to shaving district respectively by tested material, and dosage is each 0.05g·cm-2, it is administered area about 1cm2, it being given daily 3 times, medication interval is 1h, is administered the 3rd day, abrades respectively with coarse sandpaper Shaving is sentenced and is injured epidermis, has slight oozing of blood for degree.Tested material or tester 1 time, coating 10min it is coated with the most respectively in wound local After, at every Cavia porcellus wound surface, drip 0.01% histamine phosphate 0.05mL respectively, hereafter every 3min according to 0.01%, 0.02%, 0.03%, 0.04%, 0.05% progressive concentration, only it is 0.05mL/ every time, during until Cavia porcellus occurs later licking metapedes, record The total amount of every given histamine of Cavia porcellus, with this total amount as itch-threshold, and compares the itch-threshold of each treated animal.The result present invention is sprayed Mist agent and former tincture all can improve Cavia porcellus itch-threshold, the skin pruritus that suppression is caused by histamine to some extent, and present good Dose-effect dependence, and the effect of spray of the present invention is better than former tincture, with blank group comparing difference have significance (P < 0.05) 4, it are shown in Table.
Table 4 causes, on Cavia porcellus histamine phosphate, the impact reacted of itching
Note: compare with blank group#P<0.05。
Compare with former tincture group,+P < 0.05.
Experimental example 2 11-carbonyl-beta-acetyl boswellic acid (AKBA) assay
1 instrument and reagent
Waters 2695 high performance liquid chromatograph (2996PDA detector), AKBA reference substance (China's pharmaceutical biological product Calibrating institute, lot number: 111760-200601), acetonitrile (chromatographically pure, JT Baker), glacial acetic acid, methanol (analytical pure, Beijing chemical industry Factory), experimental water is prepared by Milli-Q system.Spray of the present invention (with experimental example 2);Former tincture (with experimental example 2).
2 methods and result
2.1 chromatographic conditions and system suitability
Chromatographic column: Agilent TC-C18 (4.6mm × 250mm, 5 μm);Flowing phase: acetonitrile-0.1% glacial acetic acid solution (80∶20);Column temperature: 30 DEG C;Flow velocity: 1mL min-1;Detection wavelength: 250nm;Sample size: 10 μ L.AKBA and adjacent chromatographic peak Separating degree is not less than 1.5, and number of theoretical plate is 17000.
The preparation of 2.2 reference substance storing solutions
Precision weighs AKBA reference substance 6.14mg and puts in 10mL measuring bottle, adds methanol to scale, shakes up, to obtain final product.
The preparation of 2.3 need testing solutions
The preparation of need testing solution 1: take spray of the present invention (being prepared by embodiment 1) about 0.2g, accurately weighed, put In apparatus,Soxhlet's, add methanol 80ml, reflux, extract, 9h, wash and be settled to 100ml with methanol, filter, to obtain final product.
The preparation of need testing solution 2: take former tincture (with experimental example 1) about 0.2gg, accurately weighed, put in apparatus,Soxhlet's, Add methanol 80ml, reflux, extract, 9h, wash and be settled to 100ml with methanol, filter, to obtain final product.
2.4 linear relationship precisions measure reference substance storing solution 0.25,0.5,1.0,2.0,4.0mL put 10mL measuring bottle respectively In, add methanol to scale, shake up.Precision measures each 10 μ L of above 5 parts of solution and injects chromatograph of liquid, with sample size (μ g) for horizontal Coordinate, peak area is vertical coordinate, draws standard curve, obtains regression equation: Y=1.45418 × 106X+7.42458×103(r= 0.99999) show AKBA in 0.1535-2.4560 μ g range linearly.
2.5 precision test
Taking spray of the present invention, by legal system available test sample solution 1,6 parts below " 2.3 " item, measure, result RSD is 0.67%.
Taking former tincture, by legal system available test sample solution 2,6 parts below " 2.3 " item, measure, result RSD is 0.69%.
2.6 replica tests take spray of the present invention and former tincture about 0.25g respectively, accurately weighed, by below " 2.3 " item Method makes need testing solution 1 and need testing solution 2, each 6 parts, parallel assay, results averaged, RSD=0.80% and 0.82%, show that assay method precision is good.
2.7 stability tests by legal system available test sample solution 1 below " 2.3 " item, 0,2,4,8,20h sample introduction respectively, survey It is fixed, RSD is 0.68%, shows that need testing solution 1 is stable in 20h.
By legal system available test sample solution 2 below " 2.3 " item, 0,2,4,8,20h sample introduction respectively, measure, RSD is 0.70%, show that need testing solution 2 is stable in 20h.
2.8 recovery tests take spray 0.1g of the present invention, accurately weighed, put in tool plug conical flask, and the accurate concentration that adds is 0.783mg·mL-1Reference substance solution 5mL, the more accurate methanol 20mL that adds, prepare 6 parts for examination by method below " 2.3 " item afterwards Product solution 1, measures, and results averaged, average recovery rate is 97.66%, RSD=1.36%.
Take former tincture 0.1g, accurately weighed, to put in tool plug conical flask, the accurate concentration that adds is 0.783mg mL-1Comparison Product solution 5mL, the more accurate methanol 20mL that adds, prepare 6 parts of need testing solutions 2 by method below " 2.3 " item afterwards, measure, result Averaging, average recovery rate is 97.63%, RSD=1.39%.
The mensuration of 2.9 samples precision respectively draws the need testing solution 1 and need testing solution prepared by method below " 2.3 " item 2 each 10ml, by above-mentioned chromatographic condition, according to regression equation calculation AKBA content.It the results are shown in Table 5.
Table 5 AKBA determines result
As seen from table, compared with former tincture, in spray of the present invention, the content of effective constituents A KBA of Olibanum is higher.
Detailed description of the invention:
Embodiment 1:
Prescription: Radix Trichosanthis 45g, Radix Angelicae Dahuricae 45g, Radix Aconiti Brachypodi (Radix Aconiti Szechenyiani) 34g, Borneolum Syntheticum 4g, Camphora 5g, Olibanum (processed with vinegar) 20g, vinegar system does not has Medicine 20g, Oleum menthae 10ml, Oleum Eucalypti 5ml, glycerol 35g, sodium sulfite 0.4g, disodiumedetate 0.4g and distilled water 40g。
Technique:
(1) taking Radix Trichosanthis, Radix Aconiti Brachypodi (Radix Aconiti Szechenyiani), Myrrha (processed with vinegar), the Radix Angelicae Dahuricae is ground into coarse granule, mixing, adds 80% ethanol infiltration 24 hours, then impregnate in three times with 80% ethanol, 3 hours for the first time;Second and third time each 2 hours, merges 3 impregnation liquid, filter Cross, filtrate must be mixed, standby;Take Olibanum (processed with vinegar) again, use water vapour distillation volatile oil, standby;Medicinal residues add 4 times amount The ethanol solution of 80%, reflux, extract, 2 times, each 1h, filter, merging filtrate, recovery ethanol, to only, obtains alcohol extract, alcohol extraction Take liquid and mixing filtrate merges, obtain A product;
(2) separately take Borneolum Syntheticum, Camphora, Oleum menthae, Oleum Eucalypti add 80% ethanol and dissolve, and add in A product, then add 80% ethanol and make into 1000ml, mixing, stand 24 hours, take supernatant, filter, obtain B product;
(3) take sodium sulfite and disodiumedetate is dissolved in distilled water, after dissolving, obtain C product;
(4) in C product, add B product, glycerol and above-mentioned volatile oil, stir evenly, place, filter, subpackage, to obtain final product.
Usage and dosage: external, takes and is sprayed on affected part in right amount, every day 2-3 time.
Embodiment 2:
Prescription: Radix Trichosanthis 60g, Radix Angelicae Dahuricae 60g, Radix Aconiti Brachypodi (Radix Aconiti Szechenyiani) 50g, Borneolum Syntheticum 8g, Camphora 8g, Olibanum (processed with vinegar) 30g, vinegar system does not has Medicine 30g, Oleum menthae 30ml, Oleum Eucalypti 8ml, glycerol 40ml, sodium sulfite 0.8g, disodiumedetate 0.8g and distilled water 50g。
Technique:
(1) taking Radix Trichosanthis, Radix Aconiti Brachypodi (Radix Aconiti Szechenyiani), Myrrha (processed with vinegar), the Radix Angelicae Dahuricae is ground into coarse granule, mixing, adds 85% ethanol infiltration 28 hours, then impregnate in three times with 85% ethanol, for the first time 4 time;Second and third time is each 3 hours, merges 3 impregnation liquid, filters, Filtrate must be mixed standby, standby;Take Olibanum (processed with vinegar) again, use water vapour distillation volatile oil, standby;Medicinal residues add 5 times amount The ethanol solution of 85%, reflux, extract, 3 times, each 1.5h, filter, merging filtrate, recovery ethanol, to only, obtains alcohol extract, alcohol Extracting solution and mixing filtrate merge, and obtain A product;
(2) separately take Borneolum Syntheticum, Camphora, Oleum menthae, Oleum Eucalypti add 85% ethanol and dissolve, and add in A product, then add 85% ethanol and make into 1100ml, mixing, stand 28 hours, take supernatant, filter, obtain B product;
(3) take sodium sulfite and disodiumedetate is dissolved in distilled water, after dissolving, obtain C product;
(4) in C product, add B product, glycerol and above-mentioned volatile oil, stir evenly, place, filter, subpackage, to obtain final product.
Embodiment 3:
Prescription: Radix Trichosanthis 30g, Radix Angelicae Dahuricae 30g, Radix Aconiti Brachypodi (Radix Aconiti Szechenyiani) 20g, Borneolum Syntheticum 1g, Camphora 1g, Olibanum (processed with vinegar) 10g, vinegar system does not has Medicine 10g, Oleum menthae 5ml, Oleum Eucalypti 1ml, glycerol 30ml, sodium sulfite 0.1g, disodiumedetate 0.1g and distilled water 30g。
Technique:
(1) taking Radix Trichosanthis, Radix Aconiti Brachypodi (Radix Aconiti Szechenyiani), Myrrha (processed with vinegar), the Radix Angelicae Dahuricae is ground into coarse granule, mixing, adds 75% ethanol infiltration 20 hours, then impregnate in three times with 75% ethanol, for the first time 2 time;Second and third time is each 1 hour, merges 3 impregnation liquid, filters, Filtrate must be mixed standby, standby;Take Olibanum (processed with vinegar) again, use water vapour distillation volatile oil, standby;Medicinal residues add 3-5 times The ethanol solution of amount 75-85%, reflux, extract, 0.5h, filter, merging filtrate, recovery ethanol, to only, obtains alcohol extract, alcohol extraction Liquid and mixing filtrate merge, and obtain A product;
(2) separately take Borneolum Syntheticum, Camphora, Oleum menthae, Oleum Eucalypti add 75% ethanol and dissolve, and add in A product, then add 75% ethanol and make into 900ml, mixing, stand 20 hours, take supernatant, filter, obtain B product;
(3) take sodium sulfite and disodiumedetate is dissolved in distilled water, after dissolving, obtain C product;
(4) in C product, add B product, glycerol and above-mentioned volatile oil, stir evenly, place, filter, subpackage, to obtain final product.

Claims (4)

1. a pollen is dispelled pain-easing spray of itching, it is characterised in that: by Radix Trichosanthis 30-60 part in parts by weight, Radix Angelicae Dahuricae 30- 60 parts, Radix Aconiti Brachypodi (Radix Aconiti Szechenyiani) 20-50 part, Borneolum Syntheticum 1-8 part, Camphora 1-8 part, Olibanum (processed with vinegar) 10-30 part, Myrrha (processed with vinegar) 10-30 part, and By volume Oleum menthae 5-30 part of part meter, Oleum Eucalypti 1-8 part, glycerol 30-40 part, and the sodium sulfite calculated by weight 0.1-0.8 part, disodiumedetate 0.1-0.8 part and distilled water 30-50 part are made.
2. pollen as claimed in claim 1 is dispelled pain-easing spray of itching, it is characterised in that: by Radix Trichosanthis 45 in parts by weight Part, the Radix Angelicae Dahuricae 45 parts, Radix Aconiti Brachypodi (Radix Aconiti Szechenyiani) 34 parts, Borneolum Syntheticum 4 parts, Camphora 5 parts, Olibanum (processed with vinegar) 20 parts, Myrrha (processed with vinegar) 20 parts, and by volume The Oleum menthae 10 parts of part meter, Oleum Eucalypti 5 parts, glycerol 35 parts, and the sodium sulfite calculated by weight 0.4 part, ethylenediamine tetraacetic Acetic acid disodium 0.4 part and distilled water 40 parts are made.
3. a pollen as claimed in claim 1 or 2 is dispelled the manufacture method of pain-easing spray of itching, it is characterised in that: include with Lower step:
(1) taking Radix Trichosanthis, Radix Aconiti Brachypodi (Radix Aconiti Szechenyiani), Myrrha (processed with vinegar), the Radix Angelicae Dahuricae is ground into coarse granule, mixing, adds the infiltration of 75-85% ethanol 20-28 hour, then impregnate in three times with 75-85% ethanol, for the first time during 2-4;Second and third time each 1-3 hour, merges 3 leachings Stain liquid, filters, must mix filtrate standby, standby;Take Olibanum (processed with vinegar) again, use water vapour distillation volatile oil, standby;Medicinal residues are again Add the ethanol solution of 3-5 times amount 75-85%, reflux, extract, 1-3 time, each 0.5-1.5h, filter, merging filtrate, reclaim second Alcohol, to only, obtains alcohol extract, alcohol extract and mixing filtrate and merges, obtain A product;
(2) separately take Borneolum Syntheticum, Camphora, Oleum menthae, Oleum Eucalypti add 75-85% ethanol and dissolve, and add in A product, then add 75-85% ethanol and make Become 900-1100ml, mixing, stand 20-28 hour, take supernatant, filter, obtain B product;
(3) take sodium sulfite and disodiumedetate is dissolved in distilled water, after dissolving, obtain C product;
(4) in C product, add B product, glycerol and above-mentioned volatile oil, stir evenly, place, filter, subpackage, to obtain final product.
4. pollen as claimed in claim 3 is dispelled the manufacture method of pain-easing spray of itching, it is characterised in that: comprise the following steps:
(1) taking Radix Trichosanthis, Radix Aconiti Brachypodi (Radix Aconiti Szechenyiani), Myrrha (processed with vinegar), the Radix Angelicae Dahuricae is ground into coarse granule, mixing, and adding 80% ethanol, to infiltrate 24 little Time, then impregnate in three times with 80% ethanol, 3 hours for the first time;Second and third time is each 2 hours, merges 3 impregnation liquid, filters, Mixing filtrate is standby;Take Olibanum (processed with vinegar) again, use water vapour distillation volatile oil, standby;Medicinal residues add 4 times amount 80% Ethanol solution, reflux, extract, 2 times, each 1h, filter, merging filtrate, reclaim ethanol to only, obtain alcohol extract, alcohol extract and Mixing filtrate merges, and obtains A product;
(2) separately take Borneolum Syntheticum, Camphora, Oleum menthae, Oleum Eucalypti add 80% ethanol and dissolve, and add in A product, then add 80% ethanol and make into 1000ml, mixing, stand 24 hours, take supernatant, filter, obtain B product;
(3) take sodium sulfite and disodiumedetate is dissolved in distilled water, after dissolving, obtain C product;
(4) in C product, add B product, glycerol and above-mentioned volatile oil, stir evenly, place, filter, subpackage, to obtain final product.
CN201610479159.5A 2016-06-27 2016-06-27 A kind of pollen is dispelled pain-easing spray and preparation method thereof of itching Withdrawn CN106074749A (en)

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN112826783A (en) * 2021-03-04 2021-05-25 杭州赢起贸易有限公司 Powerful mosquito-repelling itching-relieving spray and preparation method thereof

Citations (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101940631A (en) * 2010-09-20 2011-01-12 贵州弘康药业有限公司 Method for preparing pollen itching-dispelling pain-relieving tincture

Patent Citations (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101940631A (en) * 2010-09-20 2011-01-12 贵州弘康药业有限公司 Method for preparing pollen itching-dispelling pain-relieving tincture

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN112826783A (en) * 2021-03-04 2021-05-25 杭州赢起贸易有限公司 Powerful mosquito-repelling itching-relieving spray and preparation method thereof

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