| Objective:In recent years,the number of people with rheumatoid arthritis has increased significantly,and patients have to endure the problems caused by the disease.The clinical manifestations of the disease include symptoms of muscle pain,the appearance of Raynaud's sign,irregular fever,abnormalities in autoantibody blood pressure indicators,and damage of skin mucosa.Modern research has shown that Rheumatoid arthritis is one of the allergic reactions.And it is a chronic disease.The patient has a longer course and will exhibit characteristics of chronic consumption.The joint activity of the patients with rheumatoid arthritis is reduced due to joint pain.And the pain seriously hit the patient's spirit.Therefore,it is particularly important to study traditional Chinese medicine preparations to alleviate the symptoms of patients with rheumatoid arthritis.The dried cane of Piper kadsura(Choisy)Ohwi of the genus Piperaceae is Caulis Piperis Kadsurae.It belongs to drugs for dispelling wind and dampness,relieving muscle and activating collaterals.Its function is to dispell wind and dampness,relieve muscle and activate collaterals.Its indications is bruises,swelling,pain,rheumatism,chills and spasm.Modern pharmacological studies have found that the Volatile Oil from Caulis Piperis Kadsurae is anti-inflammatory and analgesic,and it has an effect on immunoregulation when absorbed into the blood.Therefore,the volatile oil extracted from Caulis Piperis Kadsurae is used for preparation.Combined with the characteristics of rheumatoid arthritis disease,the volatile Oil is prepared to be hydrogel emplastrum which will act on the joint of the patient to alleviate the patient's pain.This thesis is aimed to study the extraction process of volatile oil from Caulis Piperis Kadsurae,its chemical composition,and quality control of volatile oil.Optimize the best prescription for temperature-controlled emplastrum of Volatile Oil from Caulis Piperis Kadsurae for relieving pain.Combine the hydrogel emplastrum with the heating device can advance effect.And controling its quality is needed.Methods:(1)The optimal extraction process of volatile oil from Caulis Piperis Kadsurae was extracted by single-factor test combined with orthogonal test with extraction rate and total area of common peak as evaluation index.(2)The volatile oil from Caulis Piperis Kadsurae was extracted by the best extraction process selected.The chemical composition and the relative percentage of each component were analyzed by GC-MS.(3)The content of the active ingredient elemicin in the volatile oil from Caulis Piperis Kadsurae was determined by GC,and the quality of volatile oil from Caulis Piperis Kadsurae was controlled.(4)Establish HPLC fingerprint of volatile oil from Caulis Piperis Kadsurae,and control the quality of volatile oil from Caulis Piperis Kadsurae.(5)Determine the order of addition of the components in the hydrogel emplastrum formulation to ensure the matrix can be formed.(6)On the basis of the basic prescription,single-factor test indicated by the comprehensive sensory score(appearance traits,degree of oozing,spreadability)was conducted to examine the range of dosage of each material.(7)Determine the approximate range of each material for the prescription,and select the four most important components in the composition,the skeleton material,the cross-linking agent,the crosslinking regulator,the moisturizer,that is,NP700,hydroxyaluminum,tartaric acid,and glycerin.Set their dosage as the investigation variable of the response surface model design,and the cumulative permeation per unit area of the hydrogel emplastrum for 24h as the evaluation index.Apply the Box-Behnken response surface method to optimize the dosage of the components in the prescription.(8)Prepare with the best prescription of the hydrogel emplastrum,and combine with the heating device to obtain temperature-controlled emplastrum of volatile oil from Caulis Piperis Kadsurae for relieving pain.Then carry out visual inspection,examine the amount of paste,shape,the heat resistance and the content of the active ingredient elemicin.(9)The in vitro release of temperature-controlled emplastrum of volatile oil from Caulis Piperis Kadsurae for relieving pain was determined by a modified Franz diffusion cell method,and the in vitro release profile was drawn.Results:(1)The best extraction process for the volatile oil from Caulis Piperis Kadsurae by steam distillation is that,the material was cut into short sections,the amount of water was 5 times,the soaking time was 0.5h,and the extraction time was 6h.(2)The GC-MS determined that 35 compounds may exist in volatile oil.The identified components accounted for 52.28%of the total volatile oil.The main compounds are elemene(9.56%),2,4,5-trimethoxy-1-propenylbenzene(4.18%),?-elemene(2.03%),d-cut Alkene(2.65%),3,7,11,11-tetramethylbicyclo[8.1.0]2,6-undecene(8.65%),Pistaphos(6.13%),(1R)-(+)-?-decene(2.12%).(3)The content of elemicin in the volatile oil from Caulis Piperis Kadsurae measured by GC was 3.77%.(4)The similarity between the HPLC fingerprints of the 10 batches of volatile oil from Caulis Piperis Kadsurae and the Reference map was greater than 0.95.(5)The order of adding the paste composition of temperature-controlled emplastrum of volatile oil from Caulis Piperis Kadsurae for relieving pain is the order four.Add Sodium polyacrylate NP700 and galaluminate to the beaker,Then pour glycer into the beaker,and stir them for 10 min as phase A.Dissolve the tartaric acid in distilled water,and then add PVPK90.Stand overnight to allow PVPK90 to swell sufficiently as phase B.Phase C is a solution of volatile oil ethanol.Then add phase B and C to phase A and stir for 20 minutes.Cover it on a nonwoven fabric.(6)The single-factor test determined that the approximate dosage of the prescription substrate was sodium polyacrylate NP700 1~3g,glycolic aluminum 0.1~0.3g,tartaric acid 0.2~0.4g,glycerol 9~13 g,PVPK90 0g,distilled water 15.00g.The volatile oil was 0.19 ml and the absolute ethanol was 0.19 ml.(7)The best prescription optimized by Box-Behnken response surface method is sodium polyacrylate NP700 2.01g,glycolic aluminum 0.3g,tartaric acid 0.4g,glycerol 13g,sea buckthorn volatile oil 0.19ml,absolute ethanol 0.19 ml,distilled water 15g.The model predicted value of the cumulative drug per unit area was 17.97?g/cm~2,and the actual value was 17.91?g/cm~2.(8)Appearance inspection:The color of the paste is uniform,the softness is moderate,the thickness is uniform,the consistency is suitable.There is no particles,a few bubbles,and no oozing.And the content of the temperature-controlled emplastrum of volatile oil from Caulis Piperis Kadsurae for relieving pain is 21.14g/100cm~2.The temperature-controlled emplastrum of volatile oil from Caulis Piperis Kadsurae for relieving pain is in good shape,good heating resistance.And the content of the active ingredient of paste is 0.176 mg/g.(9)According to the fitting,the release mechanism of the hydrogel patch at 37?is most consistent with the Ritger-Peppas equation(no heating device).The release mechanism of the hydrogel patch at 47?is most consistent with the Ritger-Peppas equation(simulated with heating).Conclusion:(1)The RSD value of the extraction rate of volatile oil and the total peak area in the validation test of the best extraction process of volatile oil by steam distillation are both less than 2%,indicating that the optimal extraction process is stable and reliable.(2)The highest content of the chemical component identified by GC-MS is elemicin,and its pharmacological function is analgesic.Therefore,elemicin is regarded as an active component of volatile oil from Caulis Piperis Kadsurae.(3)The content of the active ingredient elemicin in the volatile oil from Caulis Piperis Kadsurae was determined by GC.The method has good specificity,good precision,good repeatability and good recovery.It can be used for the quality control of volatile oil from Caulis Piperis Kadsurae.(4)Establish the method of HPLC fingerprint of volatile oil from Caulis Piperis Kadsurae,which has good specificity,good precision and good repeatability,and can be used for quality control of volatile oil from Caulis Piperis Kadsurae.(5)The difference in the addition order of prescription in the sea buckwheat analgesic temperature-controlled plaster will determine whether the matrix can be formed and whether the appearance of matrix can meet the requirements.(6)The approximate amount of each component in the prescription is initially determined by the requirements of the appearance trait and the degree of ease of preparation.(7)The Box-Behnken response surface method is used to determine the optimal prescription dosage.(8)The appearance inspection,paste amount,shape and heating resistance of temperature-controlled emplastrum of volatile oil from Caulis Piperis Kadsurae for relieving pain are meet the requirements.The method for determining the content of active ingredients is reliable,accurate,and convenient to operate,and can be used for quality control of temperature-controlled emplastrum of volatile oil from Caulis Piperis Kadsurae for relieving pain.(9)The release mechanism of temperature-controlled emplastrum of volatile oil from Caulis Piperis Kadsurae for relieving pain is most consistent with the Ritger-Peppas equation.Under heating,the transdermal release of the patch has been improved.And local warming is more helpful to relieve the pain of the patient. |
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