Abstract: TLC scanning method, chloroform - methanol - benzene (2O: 1.5: O.5) as developing solvent, a measurement wavelength of 450 nm, reference wavelength of 700 nm, rhubarb pigment Determination results showed that emodin 0 The linear relationship in the range of ~1μg is good, r=O.9994, the recovery of standard addition is 99.69%, and the RSD is O.88% (n=5). This method is simple and rapid.
Key words: phlegm and blood stasis capsule; emodin; content determination; thin-layer scanning method 葶苈 血 血 胶囊 胶囊 capsule is composed of seven kinds of traditional Chinese medicines such as medlar, hawthorn and rhubarb, and there are Xuantong stagnation, Tongluo Sanjie, Xiao The function of phlegm and phlegm is mainly used for hyperlipidemia. The new drug was transferred to a new drug in 2002, the National Drug Administration of the State Drug Administration WS3-212 (X-202)-2002Z. This positive standard does not measure the content of emodin. We discussed the content of emodin in phlegm-reducing blood lipid capsules. Zui finally used thin-layer scanning method. The method is accurate, simple and convenient, and the stability, precision, reproducibility and recovery rate are ideal. This paper discusses the establishment of a method for determining emodin content.
1 Instruments and reagents
CS930 thin layer scanner (Shimadzu Corporation, Japan), silica gel G for chromatography (Qingdao Ocean Chemical Plant), emodin reference material 0756-200009 (provided by China National Institute for the Control of Pharmaceutical and Biological Products for content determination); Capsule (Jilin Tonghua Jinhui Pharmaceutical Co., Ltd.). The reagents were of analytical grade.
2 Experimental conditions
0.5% CMC-Na silica gel G plate (200 x 200 x 0.5 mm), developing solvent: chloroform-methanol-benzene (20: 1.5: 0.5), positioned under daylight.
Aspirate the reference solution, the test solution, and the negative sample solution each 4 μl, respectively, on the same carboxymethyl cellulose sodium silica gel G thin-layer plate, developed by the method, scanning at 370-700 nm, the result is large at 450 nm Absorption, while the negative sample showed no interference, so the measurement wavelength was set to 450 nm, the reference wavelength λR = 700 nm, and the scanning method was used for sawtooth scanning, SX=3, and the slit was 1.2×6 mm.
3 methods and results
3.1 Preparation of the test solution Take this product to study fine, take 1.5g precision weighing, set the Soxhlet extractor, add appropriate amount of methanol, heat reflux, extract to colorless, extract the methanol to dry, residue and water 20 ml, 2 ml of hydrochloric acid, heated under reflux for 1 h, and after cooling, extracted with diethyl ether for 6 times, 20 ml each time, and ether was evaporated at low temperature. Add the appropriate amount of methanol to the residue, transfer it to a 5ml volumetric flask, add methanol to the mark, and shake it to the test solution.
3.2 Preparation of the reference solution The emodin reference substance was added with methanol to make a solution containing 0.2 mg per 1 ml as a reference solution.
3.3 Preparation of negative sample solution According to the prescription, the other medicinal materials of rhubarb are removed. According to the preparation process, the negative blood lipid-lowering sample is prepared, and 1.5g powder is taken. According to the method under the preparation of the test solution, the negative sample solution is prepared. .
3.4 Linear Relationship Investigate the precision draw of the reference solution 1, 2, 3, 4, 5 μl on the same carboxymethyl cellulose sodium silica gel G thin-layer plate, and expand the method to determine the result, with the spotting amount as the abscissa The integral value of the absorbance is the ordinate, and the regression analysis is performed. The regression equation Y=1315.34X-7.033 is obtained, and the correlation coefficient r=0.9994.
3.5 Stability test Aspirate 2 μl of the test solution onto a thin layer of sodium carboxymethylcellulose and test it every 30 minutes. The results show that the integral value of the spot peak area is basically stable within 120 min, and its RSD=1.32 %.
3.6 Precision test The same plate precision test, according to the law, on the same thin layer board, point the same amount of the same sample, while the reference solution is 1μ1, 2μ1, according to the law, the content is determined, RSD=3.5% . In the precision test of the different plates, the same sample was placed on five carboxymethyl cellulose sodium silica gel G plates of the same size according to law, and the test was carried out after the test, RSD=2.9%. The results show that the precision is very good.
3.7 Reproducibility test According to the text method, the same batch of 010401 samples were tested 5 times independently, and the RSD=3.3%, indicating good reproducibility.
3.8 Sample recovery rate test Take batch No. 010401 sample, extract emodin content is 1.21mg/ml, take 5 parts, 5ml each, each precision added 5ml of reference solution, the concentration of reference solution is 0.5mg/ Ml, determined according to the above method, and calculated the recovery rate. The average recovery rate was 99.69%, and RSD was 0.88%.
3.9 Negative interference test Take the above test solution, negative sample solution and reference solution, and perform spectral scanning after thin layer separation according to the above conditions. The negative sample has no absorption peak at the corresponding position of the test sample and the reference substance. In the prescription, other medicinal materials other than rhubarb did not interfere with the determination of emodin content.
3.10 Sample determination The 10 μl sample was measured by the above method, and the content of emodin in the sample was calculated.
3.11 Determination of rhubarb medicinal materials The appropriate amount of rhubarb medicinal materials shall be taken and treated according to the preparation method of the test solution to determine the content of emodin.
4 Discussion This product was hydrolyzed and extracted with ether 4 times. The 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. Rhubarb has a wide production area, and the content of emodin has yet to be further explored. In summary, after the above tests, we believe that it is feasible to determine the emodin content in Qizhi Jiangzhi Capsule by TLC.
Key words: phlegm and blood stasis capsule; emodin; content determination; thin-layer scanning method 葶苈 血 血 胶囊 胶囊 capsule is composed of seven kinds of traditional Chinese medicines such as medlar, hawthorn and rhubarb, and there are Xuantong stagnation, Tongluo Sanjie, Xiao The function of phlegm and phlegm is mainly used for hyperlipidemia. The new drug was transferred to a new drug in 2002, the National Drug Administration of the State Drug Administration WS3-212 (X-202)-2002Z. This positive standard does not measure the content of emodin. We discussed the content of emodin in phlegm-reducing blood lipid capsules. Zui finally used thin-layer scanning method. The method is accurate, simple and convenient, and the stability, precision, reproducibility and recovery rate are ideal. This paper discusses the establishment of a method for determining emodin content.
1 Instruments and reagents
CS930 thin layer scanner (Shimadzu Corporation, Japan), silica gel G for chromatography (Qingdao Ocean Chemical Plant), emodin reference material 0756-200009 (provided by China National Institute for the Control of Pharmaceutical and Biological Products for content determination); Capsule (Jilin Tonghua Jinhui Pharmaceutical Co., Ltd.). The reagents were of analytical grade.
2 Experimental conditions
0.5% CMC-Na silica gel G plate (200 x 200 x 0.5 mm), developing solvent: chloroform-methanol-benzene (20: 1.5: 0.5), positioned under daylight.
Aspirate the reference solution, the test solution, and the negative sample solution each 4 μl, respectively, on the same carboxymethyl cellulose sodium silica gel G thin-layer plate, developed by the method, scanning at 370-700 nm, the result is large at 450 nm Absorption, while the negative sample showed no interference, so the measurement wavelength was set to 450 nm, the reference wavelength λR = 700 nm, and the scanning method was used for sawtooth scanning, SX=3, and the slit was 1.2×6 mm.
3 methods and results
3.1 Preparation of the test solution Take this product to study fine, take 1.5g precision weighing, set the Soxhlet extractor, add appropriate amount of methanol, heat reflux, extract to colorless, extract the methanol to dry, residue and water 20 ml, 2 ml of hydrochloric acid, heated under reflux for 1 h, and after cooling, extracted with diethyl ether for 6 times, 20 ml each time, and ether was evaporated at low temperature. Add the appropriate amount of methanol to the residue, transfer it to a 5ml volumetric flask, add methanol to the mark, and shake it to the test solution.
3.2 Preparation of the reference solution The emodin reference substance was added with methanol to make a solution containing 0.2 mg per 1 ml as a reference solution.
3.3 Preparation of negative sample solution According to the prescription, the other medicinal materials of rhubarb are removed. According to the preparation process, the negative blood lipid-lowering sample is prepared, and 1.5g powder is taken. According to the method under the preparation of the test solution, the negative sample solution is prepared. .
3.4 Linear Relationship Investigate the precision draw of the reference solution 1, 2, 3, 4, 5 μl on the same carboxymethyl cellulose sodium silica gel G thin-layer plate, and expand the method to determine the result, with the spotting amount as the abscissa The integral value of the absorbance is the ordinate, and the regression analysis is performed. The regression equation Y=1315.34X-7.033 is obtained, and the correlation coefficient r=0.9994.
3.5 Stability test Aspirate 2 μl of the test solution onto a thin layer of sodium carboxymethylcellulose and test it every 30 minutes. The results show that the integral value of the spot peak area is basically stable within 120 min, and its RSD=1.32 %.
3.6 Precision test The same plate precision test, according to the law, on the same thin layer board, point the same amount of the same sample, while the reference solution is 1μ1, 2μ1, according to the law, the content is determined, RSD=3.5% . In the precision test of the different plates, the same sample was placed on five carboxymethyl cellulose sodium silica gel G plates of the same size according to law, and the test was carried out after the test, RSD=2.9%. The results show that the precision is very good.
3.7 Reproducibility test According to the text method, the same batch of 010401 samples were tested 5 times independently, and the RSD=3.3%, indicating good reproducibility.
3.8 Sample recovery rate test Take batch No. 010401 sample, extract emodin content is 1.21mg/ml, take 5 parts, 5ml each, each precision added 5ml of reference solution, the concentration of reference solution is 0.5mg/ Ml, determined according to the above method, and calculated the recovery rate. The average recovery rate was 99.69%, and RSD was 0.88%.
3.9 Negative interference test Take the above test solution, negative sample solution and reference solution, and perform spectral scanning after thin layer separation according to the above conditions. The negative sample has no absorption peak at the corresponding position of the test sample and the reference substance. In the prescription, other medicinal materials other than rhubarb did not interfere with the determination of emodin content.
3.10 Sample determination The 10 μl sample was measured by the above method, and the content of emodin in the sample was calculated.
3.11 Determination of rhubarb medicinal materials The appropriate amount of rhubarb medicinal materials shall be taken and treated according to the preparation method of the test solution to determine the content of emodin.
4 Discussion This product was hydrolyzed and extracted with ether 4 times. The 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. Rhubarb has a wide production area, and the content of emodin has yet to be further explored. In summary, after the above tests, we believe that it is feasible to determine the emodin content in Qizhi Jiangzhi Capsule by TLC.
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