Study On Preparation Technology And Quality Control Of Luoqianyu Cataplasm

Objective: to carry out preclinical research on extraction process,preparation process,quality standard and other items by using modern science and technology and modern preparation technology according to the national registration requirements of traditional Chinese medicine compound preparation.Luoqianyu cataplasm,a Zhuang medicine,was developed into a new dosage form with large drug loading,definite curative effect,controllable quality and convenient use.Methods:(1)Extraction process: the extraction time,solvent dosage and extraction times were selected as the factors,and the yield of volatile oil,limonene,eucalyptus oil,oleoresin,etc ɑ-The contents of terpineol,methyl salicylate and n-decanoic acid were the comprehensive evaluation indexes.The optimum extraction process of volatile oil from Gaultheria Bl.var.yunnanensis(Franch.)T.Z.Hsu et R.C.Fang,Lycopodium japonicum Thunb,Lycopodium japonicum Thunb,Saraca dives Pierre and Cinnamomum burmannii(Nees et T.Nees)Bl was optimized by extraction technology.Alcohol extraction process: the amount of solvent,ethanol concentration and extraction time were taken as the investigation factors,and the factor level was selected through single factor test.The comprehensive evaluation indexes were the contents of sinomenine,zanthoxylin,tetrandrine,chlorogenic acid,polydatin,the total peak area of relative characteristic peak and the dry extract yield.Central composite design response surface methodology was used to optimize the ethanol extraction process.(2)Molding process: according to the single factor test,taking the initial adhesion,holding adhesion and sensory evaluation as the evaluation indexes,taking NP-700,silica gel powder,aluminum hydroxide,glycerin as the influencing factors,adopting the central composite design response surface optimization method,the experiment was arranged according to the central composite design of 4 factors and 5 levels,and the best molding process was selected.(3)Quality control research: to carry out the inspection of Zhuang medicine luoqianyu cataplasm’s formability,paste content and content uniformity;TLC: toluene ethyl acetate methanol water(2:4:2:1),trichloromethane methanol water(15:5:0.5),trichloromethane methanol formic acid(19:1:0.1),cyclohexane ethyl acetate formic acid(9:1.5:0.1)and cyclohexane chloroform ethyl acetate(8:1:1)were used as developing agents,and silica gel was used as stationary phase The TLC of 7 kinds of herbs were studied,including Sinomeniμm acμtμm(T h μ n b.)Rehd.et Wils.,Stephania tetrandra S.Moore,Toddali aasiatica(Linn.),D Polygonum cuspidatum Sieb.et Zucc,Boswellia carterii Birdw,Boswellia carterii Birdw,Commiphora myrrha Engl,etc.The contents of sinomenine,zanthoxylin,tetrandrine,chlorogenic acid,polydatin and dracaenin B in luoqianyu cataplasm were determined by UPLC.Results:(1)Extraction process:the best extraction process of volatile oil from luoqianyu cataplasm was to add 12 times of water for 8 hours and extract once;the best ethanol extraction process of luoqianyu cataplasm was to add 8 times of 60% ethanol for 90 minutes and extract twice.(2)Molding process: Through single factor test and central composite response surface optimization,the formulation of 1000 g blank matrix of luoqianyu cataplasm was determined as follows: np-700 60 g,silica gel powder 38 g,aluminum hydroxide 30 g,glycerin 454 g,Carbomer 940 19 g,CMC Na 19 G: edta-2 Na 1 g,water 378 G;The molding process is as follows: np-700,silica gel and aluminum hydroxide are dissolved in glycerin as a phase,edta-2na is dissolved in water,Carbomer 940 and CMC Na are added to swell as B phase,and a phase is added into B phase and stirred evenly as standby matrix;Take an appropriate amount of thick paste(5834g crude drug),add an appropriate amount of blank matrix,stir evenly,add the mixture of volatile oil,borneol,menthol,camphor and methyl salicylate dissolved in Tween-80,add blank matrix to make up to 1000 g,stir well,coat,dry at room temperature for 48 h,cover with lining,cut and package.After verification test,the surface of the formed cataplasm is smooth,no particle feeling,good skin following and uncovering,and the paste is soft with good quality;The character and shape of the product were in accordance with the relevant provisions of the Pharmacopoeia.(3)Quality control: a TLC method was established for the identification of Sinomeniμm acμtμm(T h μ n b.)Rehd.et Wils.,Stephania tetrandra S.Moore,Toddali aasiatica(Linn.),D Polygonum cuspidatum Sieb.et Zucc,Boswellia carterii Birdw,Boswellia carterii Birdw and Commiphora myrrha Engl.The results showed that the TLC method was specific,the spots were clear,and the negative had no interference.A UPLC method was established for the determination of sinomenine,nitidine,tetrandrine,chlorogenic acid,polydatin and Draconis B in luoqianyu cataplasm.The results showed that the linear range was 0.072 μg ～ 1.144 μg,0.1032 μg ～2.0064 μg,0.0288 μg ～ 0.576 μg,0.007 μg ～ 0.175 μg,0.0258 μg ～ 0.645μg and 0.0064 μg ～ 0.16 μg,respectively,and the peak area had a good linear relationship with the injection volume.The recoveries were 96.4%～ 104.8%,96.8% ～ 104.4%,92.4% ～ 102.2%,92.2% ～ 101.0%,95.45% ～103.0% and 95.4% ～ 103.3%,respectively,which were in the range of 92%～ 105%,in line with the relevant provisions of the Pharmacopoeia;The average recoveries were 100.9%,101.6%,97.3%,96.4%,102.9% and100.3%,and RSD values were 3.1%,2.9%,3.5%,2.9%,2.9% and 2.6%(n= 9),respectively.According to the determination of 10 batches of cataplasm samples,the content ranges of sinomenine,zanthoxylin,tetrandrine,chlorogenic acid,polydatin and dracaenin B were 0.254 ±0.062mg/g、0.128 ± 0.053mg/g、0.115 ± 0.413mg/g、0.430 ±0.146mg/g、1.183 ± 0.337mg/g、0.512 ± 0.082mg/g;The range of paste content is 17.26% ± 1.613g;The content uniformity was 16.16,which met the relevant requirements;The formability meets the relevant regulations.Conclusion: the preparation technology and quality standard of luoqianyu cataplasm were established,and the pharmaceutical research of luoqianyu cataplasm was preliminarily completed,which provided scientific basis for the registration and application of new drug preparation of luoqianyu cataplasm.