Novel multiple-dimension gas phase chromatographic device and analyte conveying method using multiple cooling wire connections

A technology of cooling part and connecting section, applied in the field of gas chromatography, to achieve the effect of optimizing separation conditions

Inactive Publication Date: 2007-04-25
FIRMENICH SA
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0025] In short, the chromatographic methods and devices known in the prior art are not capable of controlling the rate at which a selected peak or group of peaks (preferably spaced apart completely) elute from the second column or reach the detector. Known chromatographic methods and devices comprising automated delivery of analyte from a first separation column to a second separation column, or to a detection device such as a physical or biological detector (particularly a human nose), including thermal regulators in the analyte delivery line

Method used

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  • Novel multiple-dimension gas phase chromatographic device and analyte conveying method using multiple cooling wire connections
  • Novel multiple-dimension gas phase chromatographic device and analyte conveying method using multiple cooling wire connections
  • Novel multiple-dimension gas phase chromatographic device and analyte conveying method using multiple cooling wire connections

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Experimental program
Comparison scheme
Effect test

Embodiment

[0128] general conditions

[0129] 1. Raw materials used

[0130] Hyacinth oil was purchased from Quest International (Naarden, Netherlands), jasmine oil was purchased from Danisco (Zug, Switzerland), and lavender oil was purchased from Firmenich SA (Geneva, Switzerland). Bergamot oil was a commercially available test sample. All pure compounds were of analytical grade (>97% purity), except α-isomethylionone (>95%). α-ionone, β-ionone, (+ / -)-linalool and (-)-linalool were purchased from Fluka (Buchs, Switzerland), and α-isomethylionone was purchased from Bedoukian (Danbury, USA). ), Tetrahydroxylinalool was purchased from BASF AG (Frankfurt, Germany), Zestover  (2,4-Dimethyl-3-cyclohexene-1-carbaldehyde) was purchased from Givaudan (Vernier, Switzerland). Nonanal, terpinolene and phenylethyl alcohol were purchased from Firmenich SA. Compounds and mixtures were diluted 1:20 (v / v) with ethyl acetate (analytical grade, SDS, Peypin, France) before injection.

[0131] 2. Gas...

Embodiment 9

[0144] For the olfactometric characterization of the enantiomers, the outlet of the cryo-trap was directly connected via a fused silica "Y" connector to the FID and the same suction port as described above. The testers are spice producers. Record the onset and end times of the olfactory measurement peaks and the odor description. This experiment was repeated 3 times.

[0145] 6. Data processing

[0146] Peak heights, full width at half maximum and resolving power were calculated by Galaxie Chromatography Data System software (Varian-JMBS). The resolution between two consecutive peaks is calculated according to the following formula:

[0147] Rs = 1.18 × R t 2 - R t 1 ω 2 + ω ...

Embodiment 1

[0150] Manually Operated Connections

[0151] Very simple cryogenic control can be achieved by passing two annular columns through a T-shaped stainless steel tube as shown in Figure 2. Liquid CO 2 Inducted into the third branch of the T. Movement of the T along the double line of the column can be accomplished manually from outside the box with a rod attached to the T. Connect the two columns together using a dead-volume-free cross-tip. The cross head is connected to a flame ionization detector and a pressure controller by a deactivation capillary.

[0152] It is known that the linalool enantiomers can be separated well using a 2,6-di-O-methyl-3-O-phenyl-β-cyclodextrin column. As a preliminary test, the racemate was injected into the MDGC in the structure of Figure 4 without cryogenic trapping. The enantiomers were not separated (Figure 6B). According to the steps in Figure 4, during the second experiment, the linalool peak (Figure 6A) flowing out from the first column...

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Abstract

The invention provides a MDGC apparatus comprising a cryotrapping means capable of cooling at least twice a portion of a chemical sample and provided with detector means disposed upstream of the cryotrap and allowing identification of the said portion of the chemical sample to control the residence time of the latter in the cryotrapping means.

Description

technical field [0001] The invention relates to the technical field of gas chromatography and its use for detecting and / or separating the chemical constituents of complex mixtures of components. [0002] More specifically it relates to a new method of connecting gas chromatography (GC) columns, based on cryogenic control of analyte transport from a first column to a second column, by utilizing extremely simple connections, in order to achieve efficient multidimensional gas chromatography method (MDGC) analysis. [0003] The invention particularly relates to a device capable of carrying out the concentration of a chemical in a carrier phase (gas or fluid) moving along a column connection, using thermal regulation to vary the flow rate of the chemical. Thermal conditioning here is understood to include both cooling and heating of the chemical sample, possibly only the latter, by moving the cooling source or device along the connection after cooling the sample. [0004] The tec...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N30/12G01N30/46G01N30/02
CPCG01N30/463G01N2030/121G01N2030/025G01N30/465G01N2030/123
Inventor 阿兰·尚特罗弗雷德里克·贝诺
Owner FIRMENICH SA
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