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Planetary multi-layer helix-tube centrifugal distribution chromatograph separation apparatus

A technology of centrifugal distribution chromatography and separation device, which is applied in the field of planetary multi-layer spiral tube centrifugal distribution chromatography separation device, which can solve the problems of cumbersome operation, low separation efficiency and large equipment investment, and achieve simple operation and high separation efficiency. The effect of increasing and expanding the column capacity

Inactive Publication Date: 2004-12-01
ZHEJIANG UNIV
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  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] At present, the domestic extraction process of directly obtaining the crude extract of the alkaloid camptothecin from the natural plant camptothecin is relatively simple. Generally speaking, the purity of the crude extract product is relatively low. It can be further improved, even up to about 98%, but the yield is greatly reduced, and because the chromatography column is used, the equipment investment is large, the operation is cumbersome, and the camptothecin is easily irreversibly adsorbed on the column during column chromatography. The loss on the packing, and due to the instability of camptothecin, degradation reactions will also occur on the solid packing, so the separation efficiency is low

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  • Planetary multi-layer helix-tube centrifugal distribution chromatograph separation apparatus

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Effect test

Embodiment 1

[0015] The column capacity of the multi-layer wound polytetrafluoroethylene (PTFE) tube in the main working drum of the centrifugal distribution chromatograph of this embodiment is about 12 liters. The solvent system adopts chloroform (chloroform):methanol:water=5:2:1, and the content of camptothecin in the camptothecin crude extract is about 20% (HPLC). Take 150L of chloroform (chloroform), 60L of methanol, and 30L of water, mix them evenly in a 300L mixing kettle, and separate the upper and lower phases for later use. The above phase is used as the stationary phase, and the upper phase is pumped in at a flow rate of 50ml / min or pressed in by air pressure and filled with the working drum of the main engine. Weigh 160 grams of camptothecin crude extract, dissolve with 1000 mL of lower phase solution, and filter for subsequent use. Turn on the centrifugal distribution chromatograph, adjust the speed of the main engine to 400rpm, then pump the lower phase (the lower phase is us...

Embodiment 2

[0017] The column capacity of the multi-layer wound polytetrafluoroethylene (PTFE) tube in the main working drum of the centrifugal distribution chromatograph of this embodiment is about 25 liters. The solvent system adopts chloroform (chloroform): carbon tetrachloride: methanol: water = 2:2:3:1, and the content of camptothecin in the crude camptothecin extract is about 40% (HPLC). Take 40L of chloroform (chloroform), 40L of carbon tetrachloride, 60L of methanol, and 20L of water, and mix them in a 300L mixing kettle. After standing for stratification, separate the upper and lower phases for later use. The above phase is used as the stationary phase, and the upper phase is pumped in at a flow rate of 80ml / min or pressed in by air pressure and filled with the working drum of the host machine. Weigh 250 grams of camptothecin crude extract, dissolve with 2000 mL of lower phase solution, and filter for subsequent use. Turn on the centrifugal distribution chromatograph, adjust the...

Embodiment 3

[0019] The column capacity of the multi-layer wound polytetrafluoroethylene (PTFE) tube in the main working drum of the centrifugal distribution chromatograph of this embodiment is about 32 liters. The solvent system adopts chloroform (chloroform):methanol:0.07mol / L potassium phosphate buffer solution=3:3:1, and the content of camptothecin in the camptothecin crude extract is about 50% (HPLC). Take 180L of dichloromethane, 180L of methanol, and 60L of water, and mix them in a 500L mixing kettle. After standing for stratification, separate the upper and lower phases for later use. The above phase is used as the stationary phase, and the upper phase is pumped in at a flow rate of 80ml / min or pressed in by air pressure and filled with the working drum of the host machine. Weigh 400 grams of camptothecin crude extract, dissolve with 2500 mL of lower phase solution, and filter for subsequent use. Turn on the centrifugal distribution chromatograph, adjust the speed of the main engi...

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Abstract

Separating unit of chromatograph comprises following parts and steps: solvent system for preparing component stationary phase, mobile phase; pumping prepared stationary phase or pressing it in air pressure mode to working drum of main unit and filling up the drum with the stationary phase; running the main unit and pumping soluble crude extract of camptothecin in prearranged flux and mobile phase; based on detected spectrogram, collecting monomolecular camptothecin component from mobile phase. The two-phase solvent system is composed of hydrocarbon alkylogen, fatty alcohol and water or buffer solution of potassium phosphate under normal temperature and pressure. Upper phase is stationary phase and lower phase is mobile phase. Features of the invention are: easy of operation, small capacity of organic solvent, high efficiency. Content of product of pure monomolecular camptothecin is as high as 98%.

Description

technical field [0001] The invention relates to the field of deep processing of natural medicinal plant camptophyllum, in particular to a planetary multi-layer spiral tube centrifugal distribution chromatograph separation device. Background technique [0002] Camptothecin (CPT for short) is a five-membered ring alkaloid extracted from Camptotheca acuminata, a species of Nyssaceae (Nyssaceae) endemic to China. alkaloids. Since Wall first reported the separation, structure determination and strong antitumor activity of the alkaloid camptothecin in 1966, people have been interested in the research of the alkaloid camptothecin. Clinical application research shows that this kind of alkaloid has strong cytotoxic activity, and can inhibit DNA replication, transcription and mitosis by acting on DNA topoisomerase I (topoisomerase I, topo I), and topo I is a kind of cell An enzyme closely related to division, blocking the production of this enzyme can preve...

Claims

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Application Information

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IPC IPC(8): G01N30/00
Inventor 陈平
Owner ZHEJIANG UNIV
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