Method for separating single peak from multi-peak chromatogram

A chromatogram, a separate technology, applied in the field of stripping out individual peaks, can solve the problems of cumbersome methods, many parameters, difficult to implement, etc., and achieve the effects of simple operation, high quantitative accuracy and wide application range.

Inactive Publication Date: 2012-06-20
TIANJIN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, this method is only limited to the stripping quantification of doublets, and is powerless for the stripping quantification of multiplets
At the same ti...

Method used

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  • Method for separating single peak from multi-peak chromatogram
  • Method for separating single peak from multi-peak chromatogram
  • Method for separating single peak from multi-peak chromatogram

Examples

Experimental program
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Effect test

Embodiment 1

[0038] Instruments: HP6890 gas chromatograph, hydrogen flame ionization detector, 6890 gas chromatograph workstation;

[0039] Chromatographic column: non-polar HP-5 (5% phenylmethylpolysiloxane) column, 30m×0.32mm×2.5μm;

[0040] Conditions: The temperature of the detector is 250C, the temperature of the injection port is 250C, and the temperature of the column is 80C;

[0041] Carrier gas: Use high-purity nitrogen gas (purity not less than 99.999%), constant flow operation mode, that is, the carrier gas is at the outlet of the column, and the mass flow rate is kept constant at 1ml / min;

[0042] Injection method: split injection, the split ratio is 50:1, each injection volume is 0.2ul,

[0043] Samples: methyl tert-butyl ether, benzyl alcohol, butyric and heptanoic acids.

[0044] In order to verify the method of the present invention, the chromatograms of the above four samples are artificially superimposed with different degrees of overlap by shifting the abscissa (ie ret...

Embodiment 2

[0071] Instruments: HP6890 gas chromatograph, hydrogen flame ionization detector, 6890 gas chromatograph workstation;

[0072] Chromatographic column: non-polar HP-5 (5% phenylmethylpolysiloxane) column, 30m×0.32mm×2.5μm;

[0073] Conditions: The detector temperature is 250°C, the inlet temperature is 250°C, and the column temperature is 200°C;

[0074] Carrier gas: use high-purity nitrogen gas (purity not less than 99.999%), constant flow operation mode, that is, the carrier gas is at the outlet of the column,

[0075] The mass flow rate is kept constant at 1ml / min;

[0076] Injection method: split injection, the split ratio is 50:1, the injection volume is 0.8ul,

[0077] Samples: Isoamyl Alcohol, 1,4-Dioxane, Butyl Acetate, and Isoamyl Acetate.

[0078] Resolution: 0.44, see Figure 8 and Figure 9 .

[0079] Quantitative results:

[0080] Quantitative error of the method of the present invention: isoamyl ester (-0.32%), 1,4-dioxane (-0.81%), butyl acetate (-0.32%), ...

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Abstract

The invention relates to a method for separating a single peak from a multi-peak chromatogram. The method comprises the following steps of: performing peak shape fitting and iterative calculation, wherein the peak shape fitting comprises firstly determining a to-be-fitted single peak vertex and peak shape front edge and back edge for fitting single peak and then performing stretching change and horizontal ordinate translation according to the determined peak shape front edge and back edge, to complete peak shape fitting, and the iterative calculation comprises subtracting the overlapping peak shape of single peaks obtained by fitting from the peak shapes of multiple peaks; and repeating fitting and iterative calculation until that the error of single peak areas obtained by two adjacent iterative calculations is smaller than 0.01%, and taking the peak shape obtained in the last iterative calculation as the final single peak separated from the multi-peak chromatogram. The invention has the advantages that: the method can separate n-peak chromatograms, has a wide application range, works based on Excel office software and other computer programs with simple operation, and can control the final quantitative error not greater than 1% and ensure high quantitative accuracy.

Description

technical field [0001] The invention relates to a method for stripping individual peaks from a multiplet chromatogram. It belongs to the improved technology of chromatographic quantification and chromatographic peak shape analysis. Background technique [0002] Multiple peaks refer to the chromatographic peak shape in which the components to be separated have not been completely separated due to reasons such as high column temperature, high flow rate of mobile phase, low column efficiency or large dead volume, and the peak shapes are superimposed together. Multiple peaks are common in laboratories. Mainly with 3-5 weights. With the increasing complexity of the analyzed samples and the difficulty of optimizing the separation conditions, the overlapping phenomenon of multiple peaks in the chromatogram becomes more and more obvious. Realizing the stripping of multiple peaks has become a technical problem in chromatographic quantification and peak shape research. For the solu...

Claims

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Application Information

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IPC IPC(8): G01N30/86
Inventor 范国樑张兴华李登科
Owner TIANJIN UNIV
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