Method for preparing test solution for quality detection of safe stagnation removing preparation
A test solution and preparation technology, which is applied to the preparation field of the test solution in the quality inspection of traditional Chinese medicine preparations, can solve the problems of poor chromatographic effect, poor separation effect, poor reproducibility and the like, and achieves good chromatographic peak shape, Good effect and stable quality effect
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Embodiment 1
[0051] Remove 10g of the contents of the Jie'an capsule, add 250ml of 100% methanol by volume, sonicate for 50 minutes, let cool, filter, evaporate the filtrate to dryness, add 10ml of hydrochloric acid solution (1→5000) to dissolve the residue, centrifuge, and take the supernatant , slowly pass through a 500mg column of octadecylsilane bonded silica gel, elute with 30ml of water, collect the effluent and eluent, evaporate to dryness, add 10ml of 100% methanol by volume to the residue to dissolve, let it stand, and take the supernatant, that is For the test solution. Take stachydrine hydrochloride reference substance, add volume percentage 100% methanol to make a solution containing 10mg per 1ml, as the reference substance solution. Thin-layer chromatography method for identification of motherwort: test according to the Chinese Pharmacopoeia 2010 edition, appendix VIB thin-layer chromatography, absorb 1 μl each of the test solution and the reference solution, respectively spot on
Embodiment 2
[0054] Remove 25ml of Jie'an oral liquid, filter, evaporate the filtrate to dryness, add 5ml of hydrochloric acid solution (1→5000) to the residue to dissolve, centrifuge, take the supernatant and slowly pass it through an octadecylsilane bonded silica gel 200mg column, and elute with 15ml of water , collect the effluent and eluate, evaporate to dryness, dissolve the residue in 5ml of 95% ethanol by volume, let it stand, and take the supernatant, which is the test solution. Take stachydrine hydrochloride reference substance, add volume percentage 95% ethanol to make a solution containing 3mg per 1ml, as the reference substance solution. Thin-layer chromatography method for identification of motherwort: test according to the Chinese Pharmacopoeia 2010 edition of appendix VIB thin-layer chromatography, absorb 5 μl of the test solution and reference solution, respectively, and spot on the same silica gel G thin-layer plate, with n-butyl Alcohol-hydrochloric acid-water (8:2:1) as dev
Embodiment 3
[0056] Remove 0.5g of the contents of Jie'an capsule, add 10ml of 2% glacial acetic acid-60% ethanol solution, heat and reflux for 60 minutes, let cool, add dilute hydrochloric acid, adjust the pH to 2, filter, and pass the filtrate through 732 type sodium type cation exchange resin The column was eluted with 200ml of water and 100ml of ethanol in turn, discarded the eluent, then eluted with ammonia solution, collected the eluate, evaporated the eluent to dryness, added 1ml of hydrochloric acid solution (1→5000) to dissolve the residue, centrifuged, Take the supernatant, and slowly pass the supernatant through a 50 mg column of octadecylsilane bonded silica gel, elute with 2 ml of water, collect the effluent and eluent, evaporate to dryness, dissolve the residue with 1 ml of ethanol with a volume percentage of 70%, and let stand. Take the supernatant, which is the test solution. Take stachydrine hydrochloride reference substance, add 70% ethanol by volume percentage to make a sol
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