Method for chiral separation and measurement of methyl lactate optical isomers by capillary gas chromatography

A technology of optical isomers and gas chromatography, which is applied in the field of chiral separation and determination of methyl lactate optical isomers by capillary gas chromatography, can solve the problems of the influence of detection results and the inapplicability of target detection substances, etc.

Inactive Publication Date: 2012-11-07
CHINA AGRI UNIV
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  • Abstract
  • Description
  • Claims
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Problems solved by technology

[0008] The method for the separation of methyl lactate optical isomers by capillary gas chromatography is known, but factors such as the chiral stationary phase, the specification of the chiral chromatographic column,

Method used

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  • Method for chiral separation and measurement of methyl lactate optical isomers by capillary gas chromatography
  • Method for chiral separation and measurement of methyl lactate optical isomers by capillary gas chromatography
  • Method for chiral separation and measurement of methyl lactate optical isomers by capillary gas chromatography

Examples

Experimental program
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Effect test

Embodiment 1

[0032] Example 1: Preparation of 2,3,6-tri-O-octanoyl-β-cyclodextrin (CSP2)

[0033] Dissolve 0.3g (0.264mmol) of β-cyclodextrin in 15mL of dry chloroform, add 2.5mL of pyridine at 0°C, add 3.2mL of octanoyl chloride (21.06mmol) dropwise under ice-cooling, and stir at 0°C for 0.5h. The reaction was stirred at 60°C for 6h. After the reaction was completed, the solvent was removed under reduced pressure, dissolved in 20 mL of ice water, extracted three times with 20 mL of chloroform, the chloroform layers were combined, washed twice with saturated aqueous sodium bicarbonate solution, then washed twice with water, and finally dried over anhydrous sodium sulfate , concentrated under reduced pressure to obtain a crude product. Purification by column chromatography (toluene / ethyl acetate=1:1, v / v) gave a brown viscous product (yield 20%).

[0034] The structural confirmation data are as follows:

[0035] IR (cm -1 ): 2927, 2857 ((CH 2 , CH 3 )), 1746(C=O), 1462, 1377(CH 2 , C...

Embodiment 2

[0038] Embodiment 2, adopt capillary gas chromatography to carry out the separation of methyl lactate D, L optical isomers

[0039] 1) Preparation of capillary gas chromatography chiral column

[0040] The 2,3,6-tri-O-octanoyl-β-cyclodextrin prepared in Example 1 was used as the chiral stationary phase, and after being dissolved in dichloromethane, the wall of the stationary phase was coated on the The inner wall of the quartz capillary column was roughened with NaCl to prepare a capillary gas chromatography chiral column, and the inner wall thickness of 2,3,6-tri-O-octanoyl-β-cyclodextrin was 0.31 μm.

[0041] 2) Chromatographic conditions

[0042] Instrument: HP6890 + Gas Chromatograph, Hydrogen Flame Ionization Detector, Split / Splitless Inlet

[0043]Chromatographic column: a self-made capillary chiral column (20m × 0.25mm × 0.31 μm, long × inner diameter × inner wall thickness);

[0044] Mobile phase: high-purity nitrogen

[0045] Mobile phase flow rate: 29cm / s;

[...

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Abstract

The invention discloses a method for chiral separation and measurement of methyl lactate optical isomers by chiral capillary column gas chromatography. The preferred chromatographic conditions are as follows: chiral capillary column having inner wall coated with 2,3,6-tri-O-capryl-beta-cyclodextrin as chiral stationary phase; chromatographic column with length of 20-30 m, inner diameter of 250-320 micrometer, and stationary phase film thickness of 0.31 micrometer; inert gas as mobile phase with flow rate of 25-35 cm/s; hydrogen flame ionization detector; injection port temperature of 200-280 DEG C; detector temperature of 250-280 DEG C; and chromatographic column temperature of 50-80 DEG C. The inventive method can completely achieve baseline separation of D-methyl lactate and L-methyl lactate enantiomer chromatographic peaks, with separation degree of 5.49. The method can be utilized for simultaneous quantitative determination of D-methyl lactate and L-methyl lactate isomers.

Description

technical field [0001] The invention relates to a method for chiral separation and determination of methyl lactate optical isomers by capillary gas chromatography. Background technique [0002] Methyl lactate: chemical name is 2-hydroxypropionate methyl ester, molecular weight 104.1, molecular formula C 4 h 8 o 3 . Methyl lactate is an important organic chemical raw material and an important fine chemical, widely used in food, beverage, pharmaceutical and other industries. [0003] The optical isomers of methyl lactate are the left-handed isomer (-)-methyl lactate and the right-handed isomer (+)-methyl lactate. According to the representation method of Fisher projection formula: L-isomer (-)-methyl lactate is D-configuration, and dextro-isomer (+)-methyl lactate is L-configuration; according to the configuration representation of perspective formula: The L-isomer (-)-methyl lactate is in the R-configuration, and the dextro-isomer (+)-methyl lactate is in the S-configura...

Claims

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Application Information

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IPC IPC(8): G01N30/02G01N30/06
Inventor 史雪岩高希武宋敦伦梁沛
Owner CHINA AGRI UNIV
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