Method for separating vitamin E polyethylene glycol succinate monoester from vitamin E polyethylene glycol succinate diester

A technology of polyethylene glycol succinate and polyethylene glycol succinic acid, which is applied in the field of separation of vitamin E polyethylene glycol succinic acid mono- and di-esters, can solve unseen and complicated problems, and achieve low consumption , high degree of automation and high efficiency

Active Publication Date: 2010-06-09
ZHEJIANG UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Due to the complexity and particularity of the components of the TPGS system, there has been no report on the...

Method used

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  • Method for separating vitamin E polyethylene glycol succinate monoester from vitamin E polyethylene glycol succinate diester

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0026] Simulated Moving Bed Chromatography System C9812 (Norr, Germany), equipped with 8 chromatographic columns (ID 1×15cm), 2 in each zone, the stationary phase filled in the chromatographic column is octadecylsilane bonded silica gel, particle size 50 μm. The mobile phase was acetonitrile / isopropanol solution (50 / 50, v / v), and the temperature was 35°C. The sample used for feeding is TPGS 1000 mixed solution, concentration: 200mg / ml, wherein the monoester content is 68.3%, and the diester content is 31.4%.

[0027] A. Operating conditions:

[0028] Injection liquid flow rate: UF=1ml / min

[0029] Eluent flow rate: UD=5.7ml / min

[0030] Raffinate flow rate: U R =3.0ml / min

[0031] Extraction flow rate: U E =3.7ml / min

[0032] Switching time: t s =144s

[0033] B. Finished product analysis:

[0034] The raffinate and extract composition were analyzed by HPLC. The purity of TPGS monoester in the raffinate is 98.2%, and the yield is 99.2%; the purity of TPGS diester i...

Embodiment 2

[0036] Simulated Moving Bed Chromatography System C9812 (Norr, Germany), equipped with 24 chromatographic columns (ID 1×15cm), 6 in each zone, the stationary phase packed in the chromatographic column is octadecylsilane bonded silica gel, particle size 5 μm. The mobile phase was acetonitrile / isopropanol solution (70 / 30, v / v), and the temperature was 0°C. The sample used for feeding is TPGS 400 mixed solution, concentration: 20mg / ml, wherein the monoester content is 20.1%, and the diester content is 79.8%.

[0037] A. Operating conditions:

[0038] Injection liquid flow rate: U F =1ml / min

[0039] Eluent flow rate: U D =8.18ml / min

[0040] Raffinate flow rate: U R =3.2ml / min

[0041] Extraction flow rate: U E =5.9ml / min

[0042] Switching time: t s =180s

[0043] B. Finished product analysis:

[0044] The raffinate and extract composition were analyzed by HPLC. The purity of TPGS monoester in the raffinate is 99.9%, and the yield is 99.9%; the purity of TPGS diester...

Embodiment 3

[0046] Simulated Moving Bed Chromatography System C9812 (Norr, Germany), equipped with 32 chromatographic columns (ID 1×15cm), 8 in each zone, the stationary phase packed in the chromatographic column is octadecylsilane bonded silica gel, particle size 20 μm. The mobile phase was acetonitrile / isopropanol solution (50 / 50, v / v) at a temperature of 50°C. The sample used for feeding is TPGS 400 mixed solution, concentration: 300 mg / ml, wherein the monoester content is 55.1%, and the diester content is 44.6%.

[0047] A. Operating conditions:

[0048] Injection liquid flow rate: U F =2ml / min

[0049] Eluent flow rate: U D =21.2ml / min

[0050] Raffinate flow rate: U R =9.19ml / min

[0051] Extraction flow rate: U E =14.0ml / min

[0052] Switching time: t s =60s

[0053] B. Finished product analysis:

[0054] The raffinate and extract composition were analyzed by HPLC. The purity of TPGS monoester in the raffinate is 98.9%, and the yield is 99.9%; the purity of TPGS diest...

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Abstract

The invention discloses a method for separating a vitamin E polyethylene glycol succinate monoester from a vitamin E polyethylene glycol succinate diester. The method takes octadecyl silane bonded silica of which the grain diameter is of between 5 and 100 mu m as a stationary phase, takes a mixture of acetonitrile and isopropanol as a mobile phase, takes the mixture of vitamin E polyethylene glycol succinate of which the monoester content is of between 20 and 80 percent as a raw material, and adopts a simulated moving bed chromatographic system to separate TPGS monoester and TPGS diester of which the purity and the yield are both over 98 percent. Because simulated moving bed chromatography is a continuous operating process, the method has the advantages of high degree of automation, high efficiency, low consumption of the stationary phase and a solvent, and suitability of industrial production.

Description

technical field [0001] The invention relates to chemical separation technology, in particular to a method for separating vitamin E polyethylene glycol succinic acid mono- or di-ethylene glycol esters. Background technique [0002] Vitamin E polyethylene glycol succinate (Tocopheryl Polyethylene Glycol Succinate, TPGS) is a mixture obtained by the esterification reaction of vitamin E succinate with polyethylene glycol (PEG400-PEG 2000) of different molecular weights. From the chemical principle, two kinds of products, monoester and diester, may be generated. The TPGS mentioned now is generally considered to be vitamin E polyethylene glycol monoester. From the structural point of view, it contains both the lipophilic group of vitamin E and the hydrophilic group of polyethylene glycol long chain, so it has properties of surfactants. Due to its amphoteric nature and good water solubility, TPGS is a good non-ionic surfactant for lipophilic substances. When it forms micelles or...

Claims

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Application Information

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IPC IPC(8): B01D15/08C08G65/48
Inventor 杨亦文王靖媛鲍宗必苏宝根邢华斌任其龙
Owner ZHEJIANG UNIV
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