Identification of strong heart glycosides.

1. Preparation of the inspection solution:
take the bamboo peach leaf crush powder 3g, add 70% ethanol 40ml in a 100ml conical bottle, soak in the water bath for 5 minutes, cool,
filtration
, filter (or after treatment - method reference note 2) for identification.: The test of strong heart glycosides is carried out under strong alkaline conditions, if the sample contains tantalum, also has a red reaction, prevent the inspection, so before checking, you need to check for the use of tantalum ingredients, if there is It should be removed first, that is, ethanol leachate evaporated in the water bath, residue plus CHCl3 thermally soluble after filtration, CHCl3 liquid with 1% NaOH liquid shake, remove the crucivator, CHCl3 liquid for identification.
: clamped bamboo peach leaves or hairy yellow-clantin, often make the alcohol belt darker green, affecting the reaction. Therefore, the need to remove aerosols, the specific method is as follows:ethanol leachate in the water bath to wave off most of the ethanol (do not let ethanol evaporate), and then add water appropriate amount, so that the alcohol content of about 20%, after a little heat will be cooled, filtration, filter liquid is available for testing, or the filter liquid concentrated in the water bath to syrup, add 95% ethanol 10 ml dissolved for testing.2. Identification test:
(1) iron triclosan ice acetic acid reaction (Keller-Kiliani reaction): take alcohol or treated CHCl3 or alcohol liquid 1 ml, steamed dry on the water bath, residue dissolved in ice acetic acid 2 ml, add 1% FeCl3 ethanol liquid 1 drop, mixed evenly , pour into the
dowing
small
test tube
and then slowly add the same volume of sulfuric acid along the pipe wall, static, two liquid junction brown (glycosides), gradually turn light green, blue, and finally the acetic acid layer is all blue or blue-green (-deoxysaccharide).
(2) alkaline 3.5-dinitrobenzene reaction (Kedde reaction): take 1 ml alcohol leachate, add alkaline 3.5-dinitrobenzene
reagents
3 to 4 drops, production and red or red purple reaction.
(3) Sodium nitrostyl sodium cyanide reaction (Legal reaction): take 1 ml alcohol leachate or treated CHCl3 or alcohol solution steamed dry in the water bath, dissolve residue with 1 ml of lysate, add 0.3% nitrostyl iron cyanide solution 4 to 5 drops, mix well, and then add NaOH saturated ethanol liquid 1-2 drops, whether to show red (if the results are not obvious can take another test liquid as above operation, and finally add NaOH saturated ethanol liquid 0-5 ml, to observe whether the two-liquid interface red).
(4) alkaline bitter acid (Baljet reaction)
take sample alcohol 1 ml, add alkaline bitter acid reagent (bitter acid saturated water liquid mixed with 5% NaOH water equivalent) several drops, orange or orange red..