A kind of preparation method and product of carboxy atractylodes tripotassium salt reference substance
A technology of glycoside tripotassium salt and reference substances, which is applied in the field of preparation of chemical reference substances, can solve problems such as perishability and difficulty in separating monomers, and achieve the effects of short time consumption, high academic value, and low solvent consumption
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[0026] A kind of preparation method of carboxy atractylodes tripotassium salt reference substance according to the first aspect, comprising the following steps:
[0027] S1: First, mix Xanthium medicinal material with water, extract by cold immersion at room temperature, concentrate the liquid part after solid-liquid separation, thereby obtaining the first concentrated liquid; then, dilute the volume to 3 to 4 times the volume of the first concentrated liquid methanol was added to the first concentrated solution, precipitated, filtered, the filtrate was collected, and then concentrated to obtain the second concentrated solution; then, a saturated KCl solution whose volume was 1 to 2 times the volume of the second concentrated solution was added to the second concentrated solution In the second concentrated solution, carry out salting out, suction filtration, and collect solid; finally, use MCI column to separate the solid after salting out, wherein adopt methanol-water as eluen...
Embodiment 1
[0040] Prepare carboxy atractylodes tripotassium salt reference substance according to the following steps:
[0041] (1) Raw material extraction: crush 10 kg of Fructus cocklebur medicinal material, add 80 L of water, extract by cold soaking at room temperature twice for 2 days each time, filter with suction, combine the filtrates, concentrate to a small volume, and obtain 4000 ml of the first concentrated solution; (2) Methanol precipitation and impurity removal: add 12L methanol to the first concentrated solution, precipitate, filter, collect the filtrate, and then concentrate to 1600ml to obtain the second concentrated solution; (3) salting out: 1600ml saturated The KCl solution is added to the second concentrated solution, salted out, suction filtered, and the solid is collected; (4) MCI purification: the solid after the salted out is dissolved with 200ml of pure water and then put on the MCI column (pure water wet packing, packing It is a polystyrene synthetic resin, the ...
Embodiment 2
[0043] Prepare carboxy atractylodes tripotassium salt reference substance according to the following steps:
[0044] (1) Raw material extraction: crush 50kg of cocklebur medicinal material, add 300L of water, extract by cold soaking at room temperature twice for 2 days each time, filter with suction, combine the filtrates, concentrate to a small volume, and obtain 20L of the first concentrated solution; (2) Methanol precipitation and impurity removal: add 60L methanol to the first concentrated solution, precipitate, filter, collect the filtrate, and then concentrate to 8000ml to obtain the second concentrated solution; (3) salting out: 8000ml saturated The KCl solution is added to the second concentrated solution, salted out, suction filtered, and the solid is collected; (4) MCI purification: the solid after the salted out is dissolved with 1000ml of pure water and then put on the MCI column (pure water wet column packing, packing It is a polystyrene synthetic resin, the parti...
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