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Method for separating and purifying crude lanosterol product

A technology for lanosterol and crude products, which is applied in the field of separation and purification of lanosterol crude products, can solve the problems of poor crystal purity, low recovery rate, expensive reagents, etc., and achieve high recovery rate, good separation and good purity.

Inactive Publication Date: 2010-04-07
SHANGHAI JIAO TONG UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

The used reagent of classic bromination method is expensive, and recovery rate is low;
Master's thesis of Zhejiang University. 2005) has the disadvantages of cumbersome steps, long cycle time, low recovery rate, poor crystal purity, etc., and it needs to be repeated many times to obtain a trace amount of pure product

Method used

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  • Method for separating and purifying crude lanosterol product
  • Method for separating and purifying crude lanosterol product
  • Method for separating and purifying crude lanosterol product

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0024] 1. Weigh more than 1g of crude lanosterol on the market (see HPLC analysis) figure 1 ), add 200mL of methanol, and sonicate for 5 minutes to promote dissolution, place the suspension in a water bath at 25-35°C for 30 minutes, and the supernatant is a saturated methanol solution of crude lanosterol.

[0025] 2. Pass the above saturated solution through a 0.22 μm filter membrane as a preparative chromatographic injection solution. The inner diameter of the preparative chromatographic column is 10 mm, the column length is 250 mm, the column filler is C18 (particle size 5 μm), and the quantitative loop is 2 mL. HPLC grade methanol was used as the elution phase, isocratic elution was performed at a flow rate of 5 mL / min, and the running time was 18 minutes. By on-line UV detector monitoring fraction, detection wavelength is 210nm, according to the peak cutting and collecting effluent, lanosterol 0.65mg can be obtained, the purity is greater than 97%, and the recovery rate i...

Embodiment 2

[0030] The preparation method of lanosterol crude methanol saturated solution is the same as that in Example 1, and passed through a 0.22 μm filter membrane as the preparation of chromatographic injection solution. The inner diameter of the preparative chromatographic column is 10mm, the column length is 250mm, the filler is C18 (particle size 5μm), and the quantitative loop is 2mL. Second-rate. HPLC grade methanol was used as the elution phase, isocratic elution was performed at a flow rate of 5 mL / min, and the running time was 22 minutes. Monitor the fraction by an online ultraviolet detector, the detection wavelength is 210nm, cut and collect the effluent according to the peak, and 3.2 mg of lanosterol can be obtained with a purity greater than 97% and a recovery greater than 95%, as figure 2 shown.

Embodiment 3

[0032] The preparation method of lanosterol crude methanol saturated solution is the same as that in Example 1, and passed through a 0.22 μm filter membrane as the preparation of chromatographic injection solution. The inner diameter of the preparative chromatographic column is 10mm, the column length is 250mm, the filler is C18 (particle size 5μm), and the quantitative loop is 2mL. Second-rate. HPLC-grade acetonitrile was used as the elution phase, and the flow rate was isocratic at 5 mL / min, and the running time was 22 minutes. Fractions are monitored by an on-line UV detector with a detection wavelength of 210nm, e.g. figure 2 As shown, according to the peak cutting and collecting the effluent, 3.4mg of lanosterol can be obtained, the purity is greater than 97%, and the recovery rate is greater than 95%.

[0033] The above three examples illustrate that the strategy of repeated injection can double the growth efficiency without affecting the purity, which has important a...

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Abstract

The invention discloses a method for separating and purifying a crude lanosterol product in the technical field of the purification of organic substances, which comprises the steps of: dissolving the crude lanosterol product into an organic solvent at a temperature of between 25 and 40 DEG C through ultrasonic treatment to obtain a lanosterol solution; and filtering the lanosterol solution by a filter membrane, then using preparative high performance liquid chromatography to adopt overlapping injection for separation and purification treatment to obtain purified lanosterol. The method adopts reversed-phase high performance liquid chromatography, can ensure the characteristics of good resolution, high yield, high recovery rate, good purity and the like, can directly separate to obtain the lanosterol with the purity over 97 percent, and can be used for various sterol-related diseases and the research and development of biosynthetic pathways of various natural products. The method applies technology such as overlapping injection and linear amplification to overcome the disadvantage of low solubility caused by using reversed-phase chromatography to separate the lanosterol, uses a preparation column with the inner diameter of 20mm and the column length of 250mm, ensures that the daily preparation amount can reach near 250mg, and can meet various scientific and research requirements.

Description

technical field [0001] The invention relates to a method in the technical field of organic matter purification, in particular to a method for separating and purifying crude lanosterol. Background technique [0002] Lanosterol is an important intermediate in the sterol synthesis pathway of eukaryotic cells. In the human body, it is the synthetic precursor of cholesterol and various steroid hormones (Crit. Rev. Biochem. Mol., 34 (2), 123-140, 1999); in fungal cells, it is the precursor of ergosterol and polysteroids. An important precursor of triterpenoids with anti-cancer, anti-inflammatory, hypolipidemic and other biological activities (Nat.Prod.Rep., 15,653-696,1998; Int.Immunopharmacol.,7,701-724,2007) . Therefore, high-purity lanosterol has a very important position and role in the research of various human diseases caused by sterol metabolism and the biosynthesis mechanism of triterpenoid natural compounds. Currently commercially available high-purity lanosterol (more...

Claims

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Application Information

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IPC IPC(8): C07J9/00
Inventor 钟建江王家乐李英波
Owner SHANGHAI JIAO TONG UNIV
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