Method for preparing glycine betaine chemical reference substances from boxthorn leaves
A technology of Lycium barbarum leaves and betaine, which is applied in chemical instruments and methods, organic chemistry, cyanide reaction preparation, etc., can solve the problems of large loss in the crystallization process, cumbersome process, and no literature reports on the preparation of betaine. The effect of low cost, simple process and easy batch preparation
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Embodiment 1
[0024] Example 1 A method for preparing betaine chemical reference substances from leaves of Lycium barbarum, comprising the following steps:
[0025] ⑴Water extraction:
[0026] 1.0 Kg of Lycium barbarum leaves were dried in the shade and crushed, then added analytically pure water 4 times its mass, extracted once at 60°C for 2 hours each time, filtered and combined the filtrate A, and the filtrate A was dried under reduced pressure to a paste, that is, Brown-black solid wolfberry leaf water extract.
[0027] Wherein: the conditions of decompression drying refer to a vacuum degree of 0.06 MPa and a temperature of 70 °C.
[0028] ⑵ Silica gel column enrichment:
[0029] After the water extract of Lycium barbarum leaves was separated by silica gel column chromatography, it was eluted with 20 times the column volume of chloroform-methanol-water mixed solvent, and the fractions were collected at 1000 mL each, and detected by thin-layer chromatography, wherein the developi...
Embodiment 2
[0039] Example 2 A method for preparing betaine chemical reference substances from leaves of Lycium barbarum, comprising the following steps:
[0040] ⑴Water extraction:
[0041] 10.0 Kg of Lycium barbarum leaves were dried in the shade and crushed, then added analytical pure water 10 times its mass, extracted 3 times at 90°C for 1 hour each time, filtered and combined the filtrate A, and the filtrate A was dried under reduced pressure to a paste, that is, Brown-black solid wolfberry leaf water extract.
[0042] Wherein: the conditions of decompression drying refer to a vacuum degree of 0.09 MPa and a temperature of 50 °C.
[0043] ⑵ Silica gel column enrichment:
[0044] After the water extract of Lycium barbarum leaves was separated by silica gel column chromatography, it was eluted with 8 times the column volume of chloroform-methanol-water mixed solvent, and the fractions were collected at 2000 mL each, and detected by thin-layer chromatography, wherein the develop...
Embodiment 3
[0054] Example 3 A method for preparing betaine chemical reference substances from leaves of Lycium barbarum, comprising the following steps:
[0055] ⑴Water extraction:
[0056] 5.0 Kg Lycium barbarum leaves were dried in the shade, crushed, added analytical pure water 7 times its mass, extracted twice at 75°C for 3 hours each time, filtered and combined with the filtrate A, and the filtrate A was dried under reduced pressure to a paste, that is, Brown-black solid wolfberry leaf water extract.
[0057] Wherein: the conditions of decompression drying refer to a vacuum degree of 0.08 MPa and a temperature of 60 °C.
[0058] ⑵ Silica gel column enrichment:
[0059] After the water extract of Lycium barbarum leaves was separated by silica gel column chromatography, it was eluted with 10 times the column volume of chloroform-methanol-water mixed solvent, and the fractions were collected at 1000 mL each, and detected by thin-layer chromatography, wherein the developing solv...
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