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.
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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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