[Separation and purification of flavonoids from Smilax glabra by macroporous adsorption resin].

OBJECTIVE: To investigate the process of separating and purifying flavonoids from Smilax glabra. METHOD: With the yield of flavonoids as index, the optimum process of separating and purifying flavonoids from S. glabra Roxb was screened by static and dynamic adsorption tests. RESULT: The static saturated adsorption capacity of D101 macroporous resin to flavonoids of S. glabra was 45.6 mg x g(-1) (dry resin). The optimum conditions of dynamic adsorption and elution were as that the pH, the concentration, the adsorption velocity of the extracting solution, and the adsorption capacity were 6.00 +/- 0.20, 4.2 mg x mL(-1), 2 mL x min(-1) and 15 mL, respectively. The adsorbed resin column was washed by 100 mL 60% ethanol with pH value of 8.00 +/- 0.20 at the eluting velocity of 3 mL x min(-1) after washed by 100 mL distilled water. CONCLUSION: The flavonoids of S. glabra was able to be easily separated and purified by D101 macroporous resin under the optimum conditions above, and the recovery rate was higher than 90%. The content of obtained flavonoids reached 62.6%, which was 2 times of the content before purification.

[The optimum condition on baicalin extraction from Scutellaria baicalensis].

OBJECTIVE: To optimize the extraction process of baicalin from Scutellaria Baicalensis Georgi with ethanol. METHODS: The extraction process of baicalin from Scutellaria Baicalensis Georgi was optimized with the aid of orthogonal experiments. RESULTS: The optimal parameters were obtained as follows: extracting temperature, extracting time, ethanol concentration and mechanical stirring speed were 80 degrees C, 1 h, 60% and 400 r/min, respectively. The extracting rate of baicalin was 83.90%. CONCLUSION: Comparing ethanol circumfluence, boiling water, ultrasonic wave and semi-bionic on extracting baicalin from Scutellaria baicalensis Georgi, the ethanol circumfluence extraction is better than other technological conditions on extracting baicalin.

[Synthesis of 2-(2,5-dihydroxyphenyl)-tetraphenylporphrin and its structure identification].

2-(2,5-dihydroxyphenyl)-tetraphenylporphrin 1',2-(2,5-dihydroxyphenyl)-tetraphenylporphyrinato Cu (II)2', Ni(II)3' and Zn(II)4' were synthesized by direct reaction of 2-nitro-5,10,15,20-tetraphenylporphrin 1 or its metallic complexes 2, 3, 4 with hydroquinone under heating without solvent. The yields were about 81%, 71%, 61% and 40% respectively for 1', 2', 3' and 4'. Their structures were determined by 1H NMR, 2D NMR, IR, MS and UV-Vis spectra. It is shown that the hydroquinone connects with pyrrole ring through carbon-carbon bond, and is located in the same plane of porphyrin. One of the hydroxy group of hydroquinone is located in the deshield area of porphyrin and its proton shift occurs downfield at delta = 7.52. Another one is located in the shield area of meso benzene, and the proton shift occurs upfield at delta = 4.18. Also the 6 proton shift of hydroquinone occurs upfield at delta = 4.93.