Sanhua decoction reference sample freeze-dried powder as well as preparation method and quality detection method thereof
A quality inspection method and reference sample technology, applied in the preparation of test samples, measuring devices, instruments, etc., can solve the problems of one-by-one color development or different detection conditions, rough process, many spots, etc., to achieve effective quality control , comprehensive detection methods, and unified index components
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Embodiment 1
[0107] Embodiment 1 A kind of optimization of the preparation method of Sanhua Tang benchmark sample freeze-dried powder, comprising the following steps:
[0108] S1. Prescription dose investigation
[0109] The present invention compares three different water addition amounts of 2100ml, 2300ml and 2500ml, and finds that with the increase of water amount, such as Figure 5 , the creaming rate also increases, but the overall difference is not large, and in terms of peak output, when 2100ml of water is added, it is obviously better; so 2100ml is selected as the total amount of water.
[0110] S2. Investigation on particle size of decoction pieces
[0111] In the present invention, two kinds of sieves, 10-mesh and 5-mesh, are used to investigate the particle size of the decoction pieces: soybean size and mung bean size. image 3 and 4 , the result is that both the paste yield and the peak yield are the same. In order to reduce the loss, the size of soybean is selected for deco...
Embodiment 2
[0125] Embodiment 2 A series of methods for controlling the quality of the lyophilized powder of the Sanhua Tang benchmark sample by thin-layer chromatography, comprising the following steps:
[0126] S1. Optimization of the detection method of anthraquinones in rhubarb
[0127] (1) Optimization of the preparation of the test product
[0128] The present invention compares the different sampling amounts (1.25g, 5.0g) of the freeze-dried powder of the Sanhua Tang benchmark sample and whether it is evaporated to dryness after heating and refluxing, such as Figure 8 , it was found that taking 5.0g of the lyophilized powder of the Sanhua Tang benchmark sample, and not steaming to dryness after heating and refluxing, the spotting effect on the thin-layer board was good, so this method was used to prepare the test sample.
[0129] (2) Optimization of the spot amount of the standard solution
[0130] In the present invention, the experimental comparison is carried out on different...
Embodiment 3
[0169] Embodiment 3 adopts high performance liquid chromatography to measure the magnolol and the total content of magnolol in the freeze-dried powder Magnolia officinalis of the Sanhua Tang benchmark sample, comprising the following steps:
[0170] S1. Preparation of reference substance solution: Take magnolol and magnolol reference substance, add methanol to prepare reference substance solutions with concentrations of 60.294 μg / ml and 60.176 μg / ml respectively;
[0171] S2, the preparation of the test solution: take the 2.0g Sanhua Tang benchmark sample freeze-dried powder of Example 1 and place it in a 250ml conical flask with a stopper, add 25ml of methanol, ultrasonically treat it for 45min, and filter to obtain the test solution ;
[0172] S3. Preparation of negative sample solution: take three kinds of decoction pieces except Magnolia officinalis, prepare freeze-dried powder according to the method of Example 1, take 2.0g and place it in a 250ml conical flask with stopp...
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