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    Home > Active Ingredient News > Drugs Articles > Determination of emodin in Dingli Jiangzhi capsule by TLC scanning

    Determination of emodin in Dingli Jiangzhi capsule by TLC scanning

    • Last Update: 2007-01-31
    • Source: Internet
    • Author: User
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    Abstract: in this paper, with chloroform methanol benzene (2O: 1.5: O.5) as the developing agent, the determination wavelength is 450nm, the reference wavelength is 700nm, and the content of emodin is determined The results show that the linear relationship of emodin is good in the range of 0-1 μ g, r = o.9994, the recovery of standard addition is 99.69%, RSD is o.88% (n = 5) This method is simple and fast Key words: Dingli Jiangzhi capsule; emodin; content determination; thin layer scanning method: Dingli Jiangzhi capsule is composed of seven traditional Chinese medicines, such as Tinglizi, hawthorn, rhubarb, etc it has the functions of Xuantong Daozhi, Tongluo Sanjie and eliminating phlegm and dampness It is mainly used in hyperlipidemia In 2002, the new drug was certified as a new drug, and the national drug standard ws3-212 (x-202) - 2002z of the State Drug Administration There is no content determination of emodin in the standard We discussed the content of emodin in Dingli Jiangzhi capsule Zui finally used TLC scanning method The results of this method are accurate, simple, stable, precise, reproducible and recovery rate are ideal This paper discusses the establishment of the determination method of emodin 1 instrument and test drug cs930 thin layer scanner (Shimadzu company of Japan), silica gel G for chromatography (Qingdao marine chemical plant), emodin reference 0756-200009 (provided by China Institute of pharmaceutical and biological products for content determination); Tingli Jiangzhi capsule (Jilin Tonghua Jinhui Pharmaceutical Co., Ltd.) All reagents are analytical pure 2 Experimental conditions: 0.5% CMC Na silica gel G plate (200 × 200 × 0.5mm), developing agent: chloroform methanol benzene (20:1.5:0.5), positioning under sunlight Take 4 μ l of the control solution, the test solution and the negative sample solution, respectively, and point them on the same carboxymethylcellulose sodium silica gel G thin layer plate, develop them with the method, scan them at 370-700nm, and the results show that there is a large absorption of Zui at 450nm, but the negative sample has no interference, so the determination wavelength is set as 450nm, the reference wavelength is λ r = 700nm, sawtooth scanning with reflection method, SX = 3, and the slit is 1.2 × 6mm 3 methods and results 3.1 preparation of test solution take 1.5g of this product and weigh it accurately, put it into Soxhlet extractor, add proper amount of methanol, heat and reflow, extract to colorless, recover methanol from the extract to dry, add 20ml of water and 2ml of hydrochloric acid to the residue, heat and reflow for 1H, after cooling, extract it with ether for 6 times, 20ml each time, evaporate ether at low temperature Add proper amount of methanol to the residue to make it dissolve, transfer it to 5ml measuring bottle quantitatively, add methanol to the scale, and shake it well as the test solution 3.2 preparation of reference solution weigh the emodin reference and add methanol to make a solution containing 0.2mg/1ml as the reference solution 3.3 the preparation of negative sample solution is based on the prescription amount of other medicinal materials except rhubarb According to the preparation process, the negative sample of blood lipid reduction of Tingli is made Take 1.5g powder, and make the negative sample solution according to the method under preparation of test solution 3.4 the linear relationship was studied 1,2,3,4,5 μ l of the control solution was precisely piped onto the same carboxymethylcellulose sodium silica gel G thin layer plate, and the method was used to develop the method The results showed that the regression equation was y = 1315.34x-7.033, and the correlation coefficient was r = 0.9994 3.5 in stability test, 2 μ l of the test solution was absorbed and expanded on the carboxymethylcellulose sodium thin-layer plate The results showed that the integral value of the spot peak area was basically stable within 120 min, with RSD = 1.32% 3.6 precision test of the same plate: according to the law, point five identical test samples on the same thin plate, and point 1 μ 1 and 2 μ 1 respectively for the reference solution Operate according to the law and determine the content, RSD = 3.5% According to the different plate precision test, the same sample was selected on five carboxymethylcellulose sodium silica gel G plates of the same size according to the law After the test, RSD = 2.9% The results show that the precision is very good 3.7 in the reproducibility test, the same batch of 010401 samples were tested independently for 5 times according to the text method, with RSD = 3.3%, indicating good reproducibility 3.8 for sample adding recovery test, take the sample No 010401, the content of emodin in the extraction solution is 1.21mg/ml, take 5 parts in total, 5ml each, add 5ml each precision into the control solution, and the concentration of the control solution is 0.5mg/ml, and calculate the recovery rate according to the above method The average recovery was 99.69%, RSD was 0.88% 3.9 negative interference test take the above test sample solution, negative sample solution and control solution, after thin-layer separation according to the above conditions, carry out spectral scanning, the negative sample has no absorption peak at the corresponding position of the test sample and the control, which indicates that the content of rhubarb is not interfered by other herbs except Rhubarb in the prescription 3.10 sample determination determine the content of emodin in the sample according to the above method 3.11 determination of rhubarb content take appropriate amount of rhubarb, treat according to the method under preparation of test solution, and determine the content of emodin 4 After hydrolysis, the product was extracted with ether for 4 times, and emodin was basically extracted completely In order to be more complete, we took 6 times We have determined the content of five batches of rhubarb, but this is not enough The production area of rhubarb is wide, and the content of emodin needs further discussion In a word, through the above experiments, we think that it is feasible to determine the emodin content in Dingli Jiangzhi capsule by TLC scanning.
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