Study On Chemical Constituents Of Cistanche Deserticola in Xinjiang
Mar 08, 2022
Contact: Audrey Hu Whatsapp/hp: 0086 13880143964 Email: audrey.hu@wecistanche.com
Intro
This paper reports the analysis and identification results of fat-soluble and water-soluble components of the Orobanchaceae plant- Cistanche deserticola produced in Xinjiang by the GC-MS-DS combined method. A total of 26 components were identified and the percentage content was calculated.
Cistanche deserticola
Experiment
1. The experiment samples
The samples were collected in the Wusu area of Xinjiang in May 1986, dried in the shade, and crushed through the 20 mesh sieve. Extracted the reflux with a 2% HCl of ethanol solution, recovered the solvent under reduced pressure, concentrated the solvent to a certain volume, then adjusted it to neutral with ammonia, continued to concentrate the solvent to dry, dissolved the residue with 1% HCl and filter. The filtrate was extracted with ether. After removing impurities, it was adjusted to pH10 with ammonia and then extracted with chloroform. The chloroform was recovered from the extract under reduced pressure to obtain the fat-soluble component.
After the alkali liquor extracted by amino form was concentrated to a certain volume, then it was adjusted to pH2 with HCl and treated with Reinecke ammonium salt to obtain white crystal (yield: 0.44%) as a water-soluble component.
2. The instrument
The type of gas chromatograph was PE-sigma 2B, the quartz elastic capillary column, SE-54 (22m * 0.25mm) detector FID, and column temperature. The temperature of the injector was 260 ℃, and the split ratio was 20:1.
The type of the GC-MS-DS combined analyzer was American Finnigan MAT4510, quartz elastic capillary column SE-54 (30M * 0.25mm), and the column temperature was the same as that of gas chromatography.
Mass spectrometry identification conditions: ionization mode EI, electron energy 70eV, multiplication voltage 1.2kV., The ion source temperature was 140 ℃, and the cathode current was 0.25mA. The pressure in front of the column was 55.16kPa., The carrier gas was He. The obtained data are directly retrieved by the INCOS system of the machine, and the retrieval results would be further checked with the standard atlas in the literature to determine its structure.
Cistanche deserticola supplement
3. Results and discussion
According to the total ion flow diagram of fat-soluble components of Cistanche deserticola by capillary gas chromatography-mass spectrometry, the mass charge ratio, and relative abundance were visually compared and identified according to the mass spectrogram of peak number in the figure and the literature. The mass spectrograms of 24 components identified were intuitively consistent with the standard spectrograms in the literature. 24 kinds of fat-soluble compounds were detected, accounting for 76.01%, including 2 (3H) furanone (2.49%), 6, methyl indole (16.86%), 3-methyl-3-ethyl hexane (5.18%) - 2,6-bis (1,1-dimethyl ethyl) - 4-methyl phenol (3.63%), bicyclo [2,2,2] octyl-5-alkene-2-alcohol (2.6%), heptadecane (13.74%), 4,6-dimethyl dodecane (2.28%), 2-methyl-5-propyl nonane (3.40%), 3,6-dimethyl undecane (7.35%), and nonadecane (2.06%), eicosane (3.02%) and heneicosane (4.13), the total accounting for 66.71%.
The water-soluble crystals were dissolved in methanol and added to silica gel G chromatographic column (1.9cm * 135cm), and chloroform-methanol (6:4) was used to wash and collect the separation solution in sections, spot samples on the silica gel G thin layer, and colored with improved bismuth potassium iodide to verify its separation effect. Combined the collection solution with the same RF value and recovered the solvent under reduced pressure to obtain two kinds of white crystals. One is identified as N, N-Dimethylglycine methyl ester by MS method and the other was identified as betaine by MS and IR methods.
Cistanche deserticola supplement
