1. Extraction of complete alkaloids and also splitting up of lipophilic as well as hydrophilic alkaloids Tetrandrine is an alkaloid, as well as the plant raw material is fangji (origin). The concept of extraction as well as splitting up is the difference of greater content or primary parts and dissolution, which is called acid water percolation. The separation method is as complies with:
2. Splitting up of Tetrandrine as well as B element by reduced pressure column chromatography. Under low pressure (0.5 ～ 3kg/cm2, typically 0.3 ～ 1.2 kg/cm2), the bit diameter is between classical column chromatography (100 ～ 200μm) as well as HPLC (~ 37μm) slim layer chromatography using silica gel (or alumina) H or G (50 ~ 75μm) as a column chromatography column as a filler, its fundamental principle is the same as HPLC, and also the splitting up result is likewise in between the classic column In between as well as HPLC, the column is packed by dry technique under reduced stress, the layers are portable and also consistent, the circulation of chromatographic bands is concentrated as well as neat, and the ideal separation solvent system of thin-layer chromatography can be straight used for low-pressure column chromatography, which is a sort of splitting up. The effect is much better, the devices is basic, the procedure is convenient, and also the method is quick. Ideal for basic preparative splittings up of natural products.
( 1) Column packing
Dry packing method under reduced pressure, chromatography column specifications: column length 30cm, inner size 2cm, a total of concerning 30g of silica gel (regarding 22cm in elevation) 2.2 Blended samples and also tested to take about 150mg of acetaminophen, include a percentage of acetone to heat-dissolve (simply dissolved Include it to 1.5 g silica gel with a dropper, mix well, evaporate to dry skin on a water bathroom, grind it finely, carefully add it to the top of the column via a long-necked funnel, and also tap it up and down till the surface area of the sample is flat as well as does not stir, and then cover the empty silica gel with a height of about 1 to 2 cm, and afterwards cover with a round filter paper, as well as press it tightly.
( 2) Elution
Initial check whether the shutoffs and also pipelines from the air compressor to the chromatography column are typical, close each valve tightly, and start the air compressor to the rated pressure (5.8 kg/cm2) for usage. Use a dropper to thoroughly include a percentage of eluent (cyclohexane-ethyl formate-diethylamine/6:2:0.8) along the column wall surface of the chromatography column. When the liquid degree reaches a specific elevation, add the remainder of the eluent once more. (total concerning 250ml), quickly set up a glass common plug adapter on the top of the column, press it with an iron clamp (the adapter is punched out when anti-pressurization), very carefully open up the air compressor valve, and after that open the needle shutoff and air filter to minimize the pressure. (Note: the stress is too expensive. The glass column will take off, typically 2kg is safe, use a protective mask if essential) to mobilize the necessary stress, 0.6 ~ 1.2 kg/cm2, flow out after about 40 minutes, control the circulation rate 1ml/ Divide, one tube every 10 minutes, gather 12 to 15 components, and the entire elution process takes concerning 3 hrs.
( 3) Inspect
Each fraction was transferred to a small glass evaporator, concentrated on a water bath, and also checked by TLC. Adsorbent: silica gel G, establishing solvent: cyclohexane-ethyl acetate-diethylamine/6:3:1, changed iodine The bismuth potassium reagent was sprayed to develop color, as well as Tetrandrine and B were used as conventional controls. The exact same elements were integrated to acquire crude An as well as B, specifically, which were recrystallized with acetone and established.