苦参碱和氧化苦参碱的提取分离鉴定

• 来后打开水浴锅开关 • 仪器干燥（包括展开缸） • Add 20 ml (湿润即可) concentrated NH3. H2O to the resin
EXP. 2. Extraction ,Isolation, and Identification of Matrine and Oxymatrine
4. Procedures
(4) Alkalization of the resin and extraction of the alkaloids.
Add 20 ml (湿润即可) concentrated NH3. H2O to the resin for 15 min → transfer them to a constant pressure funnel →Extracted with 200 ml CHCl3 by reflowing for 2 hours→The extraction was dried with anhydrous sodium fulfate (Na2SO4) for 10 min and filtered→The filtrate was concentrated by air distillation→The vestigial remnant was added 20 ml acetone.
300 g×2 (2 groups) crude slices of S.flavescens was extracted with 0.5% HCl (3000 ml) for 1 day at room temperature→Add 0.1% sodium benzoate (3g)→Repeat the above procedure once again →combine the twice extract.
4. Procedures (3) Exchange of the acidic solution and precipitation reactions of the alkaloids. b. The plant extracts were tested for the presence of alkaloids with alkaloid-precipitating reactions. The precipitation reagents include dragendorff reagent
EXP. 2. Extraction ,Isolation, and Identification of Matrine and Oxymatrine
4. Procedures
(3) Exchange of the acidic solution and precipitation
reactions of the alkaloids.
碘化铋钾, silicotungstic acid硅钨酸, tannic acid鞣酸,
picric acid苦味酸 and iodine-potassium iodide (碘-碘
化钾）.
EXP. 2. Extraction ,Isolation, and Identification of Matrine and Oxymatrine
EXP 1. Preparation of Silica Gel TLC Plates 4. Procedures for Exp. 1
① It is important to ensure that the glass plates are clean and free grease before use. ② Weigh 10 g silica H and 30 ml CMC-Na (0.8%) , and mix smoothly in a 50 ml beaker. ③ Spread the slurry quickly on to the plates from one to another, and then shake the plates to form a uniform film. ④ Transfer the TLC plates to an even plane and dry it in the shade. ⑤ Activate the TLC plates at 105oC in an oven for 30 minutes. ⑥ Allow the TLC plates to cool to room temperature and store them in a desiccator.
4. Procedures (5) Detection of Matrine and Oxymatrine.
TLC plates: silica gel glass plates
Samples: the acetone solution containing alkaloids standard matrine and oxymatrine solution（回收） Developing solvents: CHCl3-MeOH (9:1) (saturated with NH3.H2O) Chromogenic agent : dragendorff reagent Compare Rf values of the sample with that of the standard matrine and oxymatrine to identify the compounds obtained.
EXP 1.
The Preparation of Thin-Layer Chromatography (TLC) Silica Gel Plates
EXP 2.
Extraction ,Isolation, and Identification of Matrine and Oxymatrine
EXP 1. Preparation of Silica Gel TLC Plates
EXP. 2. Extraction ,Isolation, and Identification of Matrine and Oxymatrine
1. Purpose Learn the methods of extracting, isolating alkaloids from the plant of Sophora flavescens Ait. and identify their structures. 2. Principle Matrine and oxymatrine from Sophora flavescens are tertracyclo- quinolizindine alkaloids, which can dissolve in dilute acidic solution to become salts.
(2) Resin Preparation
150 g cation exchange resin was soaked in 2 M HCl for 45 min→Wash to pH 5-7 with water→Soak the resin with 5% NaOH for 45 min→Wash to pH 7 with water→ Soak the resin with 2 M HCl for 45 min→Wash to pH 7 with water → store in 500 ml beaker with water and label name.
1. Purpose : Acquire the preparation of TLC silica gel plates. 2. Principle
Chromatography plates(层析板): a glass, plastic, metal sheet or plate Adsorbents(吸附剂): Silica gel H, silica gel G, silica gel GF254, silica gel HF254, aluminum oxide, polyamide and cellulose Adhesives(粘合剂): CMC-Na, Plaster of Paris (CaSO4.1/2H2O), starch(淀粉） Activity grade: five grades
EXP. 2. Extraction ,Isolation, and Identification of Matrine and Oxymatrine 4. Procedures (1) Extraction of matrine and Oxymatrine from S. flavecens.
EXP. 2. Extraction ,Isolation, and Ide来自百度文库tification of Matrine and Oxymatrine
EXP. 2. Extraction ,Isolation, and Identification of Matrine and Oxymatrine
EXP. 2. Extraction ,Isolation, and Identification of Matrine and Oxymatrine
2. Principle Pass the solution through a column of cation exchange resin (H+ type), which will absorb the alkaloids, then the resin was alkalified with concentrated NH3· 2O and the alkaloids H mixture is extracted with CHCl3. Principle of strong acidic cation exchange resin RSO3-. Na+ + HCl → R-SO3-. H+ + NaCl RSO3-. H+ + [BH]+. Cl- → RSO3-. [BH]+ + HCl RSO3-. [BH]+ +NH3· 2O → RSO3-. [NH4]+ + B- + H2O H 3. Apparatus and Reagents Amberlite IRC-50, Constant pressure funnel, et al.
a. The extraction was filtered and passed through
the prepared resin（flow rate) (the exchanging end point was detected by dragendorff reagent) →Wash the resin to pH 5-7 with water→Then the resin was vacuum filtered and put into a paper box for open-
Moisture content Activity grade 0 Ⅰ 5 Ⅱ 15 Ⅲ 25 Ⅳ 38 Ⅴ
Adsorption-------Partition
3. Apparatus and Reagents
– Glass plates 5×10 (5) or 2.5×7.5 cm (10), clean and dry – silica H for TLC – 0.8% CMC-Na
air drying and label name.
EXP. 2. Extraction ,Isolation, and Identification of Matrine and Oxymatrine
EXP. 2. Extraction ,Isolation, and Identification of Matrine and Oxymatrine