Method for determining methyl lactate optical isomer based on capillary gas phase chromatogram chiral separation

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

Inactive Publication Date: 2012-10-31
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, the column temperature of the chromatographic column, the split ratio, and the flow rate of the mobile phase have great influence on the detection results. Has a large effect, or is not suitable for target detection

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  • Method for determining methyl lactate optical isomer based on capillary gas phase chromatogram chiral separation
  • Method for determining methyl lactate optical isomer based on capillary gas phase chromatogram chiral separation
  • Method for determining methyl lactate optical isomer based on capillary gas phase chromatogram chiral separation

Examples

Experimental program
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Embodiment 1

[0032] Example 1: Preparation of 2,3,6-tri-O-pentanoyl-β-cyclodextrin

[0033] Dissolve 0.3g (0.264mmol) of β-cyclodextrin in 15mL of dry chloroform, add 2.5mL of pyridine at 0°C, add 2.5mL of valeryl 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 ): 2958, 2930, 2872 (CH 2 , CH 3 ), 1740 (C=O), 1462, 1380, 1343, (CH ...

Embodiment 2

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

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

[0040] The 2,3,6-tri-O-pentanoyl-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-pentanoyl-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 × 0.31μm, long × inner diameter × inner wall thickness);

[0044] Mobile phase: high-purity nitrogen

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

[0046] Inl...

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Abstract

The invention discloses a method for separating and detecting methyl lactate optical isomers. In the method for separating and detecting the methyl lactate optical isomers, the capillary gas phase chromatogram chiral separation method is adopted, and the preferable chromatogram conditions are as follows: a capillary chiral column taking wall coated 2,3,6-tri-O-valeryl-delta-cyclodextrin as a chiral stationary phase is adopted; a chromatogram column has the length of 20m-30m and the internal diameter of the chromatogram column is 250mum-320 mum, and a stationary phase film in the chromatogram has the thickness of 0.31mu m; a mobile phase adopts inert gases, and the flow velocity is 25-35cm / s; a detector is a hydrogen flame ionization detector; the temperature of a sample feeding port is 200-280 DEG C; the temperature of the detector is 250-280 DEG C; and the temperature of the chromatogram column is 50-80 DEG C. By using the determination method, the baseline separation of the chromatogram peaks of methyl lactate D, L enantiomers can be achieved with the separating degree reaching 6.08; and the method can simultaneously be used for the quantification of the methyl lactate D, L enantiomers.

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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Patent Type & Authority Applications(China)
IPC IPC(8): G01N30/88G01N30/60
Inventor 史雪岩高希武宋敦伦梁沛
Owner CHINA AGRI UNIV
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