2.2 The linear relationship of the test accurately weighed the amount of puerarin reference substance dried to constant weight, dissolved with 30% ethanol solution, made of each lml containing 00! The puerarin reference solution, precision pipette 1, 2, 3, 4, and 111, respectively, was placed in a 11111 volumetric flask, diluted with 30% ethanol to the mark, and 10 μf/l was sampled under the above chromatographic conditions, and the integrated value was measured. The linear regression calculation gives the equation 丫=3.717914-1.319 103, r=0.9997. The linear relationship is good.
2.3 precision experiments accurately draw O.OlVml puerarin reference substance lOf, according to the above chromatographic conditions repeated injections 5 times, the results show that the method has a good precision. See Table 1 Table 1 Precision Test Results 2.4 Reproducibility Test Take the same batch of cold heat particles, using this method to operate 5 times, the results show that the method has good reproducibility. See Table 2 Table 2 Test results of liquidity 2.5 Stability test Take the same test solution, set it in a brown volumetric flask and measure it at 2, 4, 6, and 8h. The result shows that it can be measured within 8 hours. See Table 3 Table 3 Results of the qualitative fruit determination time h Integral value 2.6 Recovery test Precision weighed puerarin reference substance was added to the known content of the sample, according to the sample below the determination item is not determined, calculate the recovery rate, the results in Table 4. Table 4Recovery rate test results Average recovery rate 3 Including assay 3.1 Preparation of control solution Accurately weigh the dried puerarin reference substance into a volumetric flask, add 30% ethanol solution to dissolve and dilute to the mark. Each 1 ml of a puerarin solution containing O.Olftng/ml was prepared.
3.2 Preparation of sample solution Take cold heat-removing particles 10g, and study carefully. Take lgf|Medium, set stoppered Erlenmeyer flask, accurately add 30% ethanol 50ml, Weigh, ultrasonic (power 250w, frequency 33kHz) 20min, let cool, then use 30% ethanol to make up for lost weight, shake , Filtration using a microporous membrane, continuous filtrate.
3.3 Each precision absorbs the above two solutions lOxl, injected into the high performance liquid chromatograph, determine the peak area integral value calculation, that is, too. See Table 5 Table 5 Sample Content Determination Results in Batch No. Content mg/g Average mg/g 4.1 Determination of the extraction method for the test sample. The residue extracted according to the above method was added with 50 ml of 30% ethanol and the sonication was continued for 20 min. Allow to cool, weigh, replenish with 30% ethanol to lose weight, and filter with a microporous membrane. The continuous filtrate injection 101 showed no corresponding peak at the corresponding position of the puerarin reference substance. Therefore, it is considered that the above-described sample extraction method can completely extract the puerarin in the sample.
4.2 The origin of the raw materials of traditional Chinese medicine is different, and there are some differences in the content of cold heat-removing particles of different batches. Therefore, the lower limit of one content can be measured in multiple iterations to control its quality standard.
