Study On The Quality Standard Of Zhipiantong Tablets

Zhipiantong tablet is a kind of compound preparation which is composed of eight traditional Chinese medicines of paeoniae alba,rhizoma ligustici wallichii,angelica dahurica,liquorice,white mustard seed,radix bupleuri,bunge cherry seed,aroma.Zhipiantong tablet is used in the treatment of vascular headache and all kinds of migraine,and have the effect of activating blood,functions of relieving pains,this experiment had searched by thin layer chromatography(TLC)to the prescriptions of radix paeoniae alba,radix angelicae,rhizoma ligustici wallichii,liquorice,white mustard;in order to determine the corresponding quality criteria and the control indicators,high performance liquid chromatography(HPLC)method for active ingredients was used in the prescription,the content of paeoniflorin in linear range for the paeoniflorin investigation,the specificity test,precision test,repeatability test and stability test,recovery rate test,through the two aspects of qualitative and quantitative research to treat in order to determine the corresponding quality criteria and the control indicators,pain quality meets the standards.In addition,we carried on the preliminary stability test,accelerated test and long-term test,influence factors,including high temperature,light,humidity,etc.).The experimental results were as followed:(1)The preparation of medicines:according to the prescriptions of weigh and rhizoma ligustici wallichii,radix bupleuri,bunge cherry seed,sweet,angelica dahurica,crushed into the meal,according to extract and extract diacolation method under version of "China pharmacopoeia"(2015 four general principles of the preparation of 0189),through the ethanol impregnation after 24 h,then with ethanol diacolation 24 h,velocity as per kilogram of 3～5 ml per minute,diacolation liquid recovery after ethanol,the reduced pressure concentration,concentration and density of 1.20～1.30 clear cream(50℃ hot test),put aside;More than the rest of the radix paeoniae alba,white mustard,liquorice and 5 herbs liquid mixture,then add water,add water 2 times,first add 10 times the amount of water,twice with eight times the amount of water,decoction and decoction could be 2 h at a time.Incorporating two decoction decoction,the reduced pressure concentration and density of 1.20～1.30)(50℃ hot test of paste,then add ethanol,the alcohol content of 75%,the precipitation 48 h,then take the supernatant,after the recovery of ethanol,the reduced pressure concentration,concentration and density of 1.20～1.30 cleaning cream(50℃ hot test);Incorporating these two clear cream,add the right amount of auxiliary materials,mixing,granulating,drying,add sodium carboxy methyl starch,blending,tablet and package film,for a quick cure slant pain.The partial pain tablet weight variation,disintegration time limit,the microbial limit inspection,were all qualify the rules.(2)The qualitative identification:the study had made in the five traditional Chinese medicine(TCM)by thin layer chromatography(TLC)for qualitative identification.First of all,according to the experiment requirement,The preparation of the test solution,reference substance solution and the negative contrast solution,according to the thin layer chromatography(TLC)(2015)0502 "China pharmacopoeia" four rules)on five traditional Chinese medicine identification,we had searched through the thin layer chromatogram.(3)Content determination:using high performance liquid chromatography(HPLC)method to determine the paeoniflorin content,and the selected chromatographic conditions were:filling agent for octadecyl silane bonded silica gel,in acetonitrile-water-phosphate(14:86:0.1).as mobile phase and detection wavelength of 230 nm,column temperature 25℃,flow rate 1.00mL·min-1,10 ul sample quantity.Preparing the test samples corresponding solution,reference substance solution,negative control solution to determine the content of paeoniflorin,then investigates methodology including linear range,precision of test,repeatability test and stability test,the specificity test,recovery test and so on,then we got the corresponding chromatograph chart,the experimental results proved that the product precision had good repeatability,and other experimental results were also conformed to the requirement of pharmacopoeia.Finally draw the conclusion:in the qualitative identification,strictly in accordance with the provisions of the new pharmacopoeia,this product was mixed in traditional Chinese medicine on thin layer chromatography(TLC)identification,chromatogram proved that this product contains the five traditional Chinese medicine.Content determination by high performance liquid chromatography(HPLC)method,the results complyed with the provisions of the state pharmacopoeia.In the study of methodology,paeoniflorin in six including 6g/ml～36 including g/ml,within the scope of concentration,concentration and peak area linearly were related,by observing the chromatogram could see negative reference substance solution in the test solution and reference substance in the solution of paeoniflorin retention time on the corresponding position without absorption peak appears,experiments showed that the negative control without interference,and had a good specificity of this method.In accordance with requirements of the new drug research and development,the partial pain tablet carried on the preliminary stability test,accelerated test and long-term test,and the influence factors such as high temperature,light,humidity.By influencing factors,including high temperature,light,humidity,etc.)The experimental results showed that the product under the condition of high temperature and high humidity stability;In light(4500 Lx-500 Lx)under the condition of character for the class flake tan ten days,had no obvious change,and other indicators showed that the quality of light was not stable;Pharmaceutical packaging material under strong light irradiation(4500 Lx-500 Lx)properties unchanged.By accelerating test,this product had for 3 months and 9 months of long-term test,the test results showed that each index all did not change obviously.We had certified that the sample process had the stability and feasibility of prescription,and the selection of packaging materials was suitable for this product.