Quality detection method for Liangfu pill-like preparations
A quality inspection method, the technology of Liangfu pills, applied in the direction of measuring devices, instruments, scientific instruments, etc., can solve the problems of not representing functions and indications, the quality of difficult preparations, etc., and achieve good separation, high environmental adaptability, and quality assurance. Effect
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Embodiment 1
[0047] 1. Preparation of reference substance solution: Take an appropriate amount of reference substance of galangin, kaempferone, citronone, α-cyperone, and cyperenone, and add methanol to make a solution containing 1 mg per 1 mL, as the reference substance solution .
[0048] 2. Preparation of the test solution: Take 1 g of Liangfu pill powder, add 25 mL of methanol, sonicate for 30 minutes, filter, evaporate the filtrate to dryness, add 1 mL of methanol to dissolve the residue, and use it as the test solution.
[0049] 3. TLC conditions:
[0050] Developing agent: petroleum ether (60-90°C)-ethyl acetate (5:1);
[0051] TLC: Silicone GF 254 plate;
[0052] Sample volume: 4 μL each for the test solution and the reference solution;
[0053] The temperature was 22°C and the relative humidity was 58%.
[0054] 4. Inspection: inspect under the ultraviolet lamp 254nm, the result is as follows figure 1 As shown, the spots of each index component are obvious and separated well; ...
Embodiment 2
[0071] Embodiment 2 extraction method investigation
[0072] Take 1g of Liangfu pill powder, add 25mL of methanol, investigate the two extraction methods of reflux extraction and ultrasonic extraction respectively, the extraction time is 30min, filter, the filtrate, evaporate to dryness, add 1mL of methanol to the residue to dissolve, as the test solution, TLC Chromatographic conditions and inspection methods are the same as in Example 1, and the results are as follows Figure 9 and Figure 10 shown.
[0073] The results show that the main spots are clearer in both extraction methods. Because the operation of the ultrasonic extraction method is simpler and more convenient, the preferred ultrasonic extraction method is used as the preparation method of the test sample in the present invention.
Embodiment 3
[0074] Example 3 point sample volume investigation
[0075] According to the method of Example 1, the same silica gel GF254 thin-layer plate was taken, and the sample volumes of 1, 2, 4, 6, 8, and 10 μL were investigated respectively. The result is as Figure 11 and Figure 12 shown.
[0076] The results showed that when the spotting volume of the test solution was 2-10 μL, the clarity and separation of the spots were better, and the optimum spotting volume was 4 μL.
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