A method for rapid detection of phenyllactic acid isomers by reversed-phase high performance liquid chromatography

A reversed-phase high-performance liquid phase, phenyllactic acid technology, applied in the field of high-performance liquid chromatography analysis, can solve the problems of poor use, extensive capillary electrophoresis, and no preparation conditions, etc., to achieve simple operation, rapid detection, and good reproducibility Effect

Inactive Publication Date: 2011-12-21
JIANGNAN UNIV
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  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Although capillary electrophoresis has a good separation of its optical isomers, compared with high performance liquid chromatography, it is not as widely used as the latter and capillary electrophoresis can only be used for analysis and does not have the conditions for preparation

Method used

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  • A method for rapid detection of phenyllactic acid isomers by reversed-phase high performance liquid chromatography
  • A method for rapid detection of phenyllactic acid isomers by reversed-phase high performance liquid chromatography
  • A method for rapid detection of phenyllactic acid isomers by reversed-phase high performance liquid chromatography

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0022] Example 1 Detection of L-(?)-3-phenyllactic acid standard sample

[0023] Use L-(?)-3-phenyllactic acid from Sigma Company to prepare a standard solution with a concentration of 1 mg / mL with distilled water or mobile phase solution, and take a certain volume of this solution for detection and analysis by high performance liquid chromatography. The high performance liquid chromatography conditions are: the model of the high performance liquid chromatography is Shimadzu LC-20AT; the model of the chromatographic column is inertsil ods-sp; The liquid:methanol volume ratio is 90:10, the flow rate is 1mL / min, the column temperature is 30°C, the sample volume is 20μL (concentration 1mg / mL), and the detection wavelength is 254nm.

[0024] figure 1 It is the detection result graph of L-(?)-3-phenyllactic acid standard sample. The retention time of L-(?)-3-phenyllactic acid under this chromatographic condition is about 16.825min. The peak area of ​​L-(?)-3-phenyllactic acid is ...

Embodiment 2

[0025] Example 2 Detection of D-(+)-3-phenyllactic acid standard sample

[0026] Use D-(+)-3-phenyllactic acid from Sigma Company to prepare a standard solution with a concentration of 1 mg / mL with distilled water or mobile phase solution, and take a certain volume of this solution for detection and analysis by high performance liquid chromatography. The high-performance liquid chromatography conditions are: the model of high-performance liquid chromatography is Shimadzu LC-20AT; The volume ratio of buffer solution:methanol is 90:10, the flow rate is 1mL / min, the column temperature is 30°C, the sample volume is 20μL (concentration 1mg / mL), and the detection wavelength is 254nm.

[0027] figure 2 It is the detection result graph of D-(+)-3-phenyllactic acid standard sample. The retention time of D-(+)-3-phenyllactic acid under this chromatographic condition is about 19.017min, and the peak area of ​​D-(+)-3-phenyllactic acid is calculated by the integration software, and the...

Embodiment 3

[0028] Example 3 Detection of DL-3-phenyllactic acid standard sample

[0029] Use DL-3-phenyllactic acid from Sigma Company to prepare a standard solution with a concentration of 1 mg / mL with distilled water or mobile phase solution, and take a certain volume of this solution for detection and analysis by high performance liquid chromatography. The high-performance liquid chromatography conditions are: the model of high-performance liquid chromatography is Shimadzu LC-20AT; The volume ratio of buffer solution:methanol is 90:10, the flow rate is 1mL / min, the column temperature is 30°C, the sample volume is 20μL (concentration 1mg / mL), and the detection wavelength is 254nm.

[0030] image 3 It is the detection result chart of DL-3-phenyllactic acid standard sample. The retention time of L-(?)-3-phenyllactic acid is about 16.908min under this chromatographic condition, and the retention time of D-(+)-3-phenyllactic acid is about 19.108min under this chromatographic condition. ...

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Abstract

The invention relates to a method for analyzing DL-3-phenyllactic acid enantiomer by a reversed phase high performance liquid chromatogram and belongs to the technical field of high performance liquid chromatogram analysis. The method comprises the following steps of: dissolving cyclodextrin into buffer solution to obtain cyclodextrin buffer solution containing a chiral selective agent; dissolving a sample into distilled water or the cyclodextrin buffer solution; and separating two enantiomers of D-(+)-3-phenyllactic acid and L-(-)-3-phenyllactic acid by the reversed phase high performance liquid chromatogram. The cyclodextrin serves as a chiral agent, is low in background absorption, low in price and readily available, and adopts a reversed phase C18 chromatographic column commonly used in the liquid chromatogram instead of an expensive chiral chromatographic column. Compared with the prior art, the method has the advantages of low detection cost, high separation efficiency, high detection sensitivity, no toxicity and low consumption of the reagent, environment friendliness, simpleness and convenience for operation, and capacity of realizing chiral separation of the enantiomers under the inversed phase condition. By the method, the medicine synthetical intermediate DL-3-phenyllactic acid enantiomer can be detected rapidly and the produced phenyllactic acid can be detected qualitatively and quantitatively.

Description

technical field [0001] The invention relates to a rapid detection method for isomers of phenyllactic acid by reverse-phase high-performance liquid chromatography, and the invention relates to a rapid chiral analysis method for optically pure L-type and D-type phenyllactic acid of pharmaceutical synthesis intermediates and food preservatives. It belongs to the technical field of high performance liquid chromatography analysis. Background technique [0002] Phenyllactic acid (2-hydroxy-3-phenylpropionic acid) is a substance produced by lactic acid bacteria, which has broad-spectrum antibacterial properties and can inhibit a variety of food-borne pathogens (such as pathogenic Escherichia coli, single monocytogenes and Staphylococcus aureus) and spoilage bacteria (ochrax, verrucosporine, and penicillin). Therefore, phenyllactic acid is a new type of antibacterial substance that can be used in food systems after lactic acid, acetic acid, and nisin. In addition to applications i...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N30/02
Inventor 徐学明徐进赵文秀杨哪金征宇
Owner JIANGNAN UNIV
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