A Preliminary Study On The Chemical Constituents Of Cistanche Deserticola in Xinjiang

Contact: Audrey Hu Whatsapp/hp: 0086 13880143964 Email: audrey.hu@wecistanche.com

Intro

Cistanche salsa (C.A.Mey.) is the fleshy stem of Cistanche deserticola, also known as Grand Rue, longitudinal Rue, and Ground Sealwort. It is distributed in the desert Gobi area. It is also known as "desert ginseng" because it has the functions of benefiting the kidney, strengthening the Yang, tonifying essence and blood, prolonging life, and so on. Japanese scholars have studied and reported the chemical constituents of Cistanche deserticola in Inner Mongolia, but there is no report on the chemical constituents of Cistanche deserticola in Xinjiang. To study and compare Cistanche deserticola, Xinjiang Medical College has done some work to extract and separate chemical components from the herbs of Cistanche deserticola purchased by the medicinal Station in this area and obtained two kinds of crystals, namely Crystal I, Crystal II, and some white solid powder. Crystal I is identified as D-Mannitol and Crystal II as β-Sitosterol by melting point determination, infrared spectroscopy, thin-layer chromatography, and standard reference methods, but the white solid powder was not further identified due to its little amount.

Experimental part

The melting point was measured by the X4 micro melting point tester, and the thermometer was not calibrated. The infrared spectrum is IR-440 infrared spectrophotometer (Shimadzu), potassium bromide tablet pressing method. The type of centrifugal thin layer chromatography is LBC-1. Silica gel for the column layer was produced by Qingdao marine chemical plant, and ethanol for elution was medicinal ethanol. After re-distillation, other solvents are chemically pure or analytical pure. The Cistanche herbs are purchased from Changjizhou medicinal materials company.

1. Extraction and separation

The herbs were processed into coarse powder from the 2kg of Cistanche crude medicine, put into a Soxhlet extractor, and heated with methanol for reflux extraction. The methanol solution is concentrated under reduced pressure to obtain the extract, and a white solid was separated from the extract, and Crystal I was obtained by repeated recrystallization with ethanol. The remaining extracts were extracted with petroleum ether, ethyl acetate, and n-butanol many times. After the acetic acid and acetic acid are concentrated under reduced pressure, the column layer is separated with silica gel (100 mesh ~ 160 mesh), eluted with chloroform and ethanol mixed solvent (the proportion of ethanol gradually increases), and a total of 200 fractions are collected, about 80ml per fraction. Among them, 89-90 fractions were combined and concentrated and recrystallized with ethanol to obtain one white powdery solid, 48-50 fractions were combined and concentrated to obtain waxy solid (about 2.2g), and crystal II was obtained by centrifugal thin-layer separation. The centrifugal thin layer separation conditions are as follows:

Injection volume: 0.55g, dissolved in 4ml CH2Cl2:

Adsorbent: silica gel GF, thickness 2mm

Eluent: n-hexane: 120ml, ethyl acetate (8:2), n-hexane: ethyl acetate (5:5) 80ml

Eluent flow: rate 5ml / min

Separation time: 40 minutes

A total of 15 fractions (about 12ml per fraction) were collected from the separation results, of which 4-6 fractions were placed to precipitate white acicular crystals, namely Crystal II.

2. Appraisal

Crystal I is a white acicular crystal with a melting point of 169-171 ℃, mixed with D-Mannitol standard, melting point measurement, the melting point does not decrease. It is close to the literature value of D-Mannitol. The infrared spectrum was also consistent with the D-Mannitol standard. Crystal I was identified as D-Mannitol.

Crystal II, white acicular crystal, melting point 139-141 ℃, mixed β-Sitosterol standard, and determined the melting point of the mixture, the melting point of the mixture did not decrease. The Infrared spectrum of Crystal II and the Infrared spectrum of β- Sitosterol standard are completely consistent. The product was red-purple in reaction with concentrated sulfuric acid vinegar, dark blue in reaction with 10% phosphomolybdic acid, and dark brown in reaction with vanillin reagent. Crystal II was identified as β- Sitosterol.

White powdery solid was red-purple in reaction with concentrated sulfuric acid vinegar, α- Naphthol test was positive and insoluble in 5% sodium hydroxide solution. Due to the small quantity, no further identification could be made.

Reference

1. Dictionary of traditional Chinese medicine (Volume I), compiled by Jiangsu new medical college, Shanghai People's publishing house, 1977, 896

2. Yang Xiuwei. Study on chemical constituents of anti-aging traditional Chinese medicine Cistanche. Information on traditional Chinese medicine, 1985; 2:31

3. Kobayashi Hiromi, Komatsu Junko. Journal of Pharmacy (Japanese) 1983; 103(5)508

4. Kobayashi H, et al. Chem Pharm Bull 1984; 32(5):1729

5. Merck Index. Ed 9.745.