JP3174671U - Smell sniffer-gas chromatograph mass spectrometer - Google Patents

Abstract

The present invention provides an odor-gas chromatograph mass spectrometer capable of separating components of a sample with high accuracy and simultaneously analyzing the chemical structure and “odor” of each component.
A database in which compound names, mass spectra, retention indices, odor quality and threshold values are registered by analyzing known odor components in advance, and a chromatograph that separates and develops components in a sample having odors in the time direction. And a mechanism for displaying the chromatogram obtained by the chromatograph means, and from the database information of the component selected before the sample measurement, a notice for notifying the peak position of the chromatogram display mechanism A mechanism was provided.
[Selection] Figure 1

Description

  The present invention is a scent-gas chromatograph mass spectrometer (hereinafter referred to as a scent-sniff-GC-MS device) that can separate components of a sample with high accuracy and simultaneously analyze the chemical structure and “odor” of each component. About.

  In recent years, various products have been developed in the field of food and daily necessities, and research on qualitative analysis and quantitative analysis for "odor" has been attracting attention. In environmental analysis, demand for off-flavor / bad odor analysis is increasing.

  Conventionally, the identification and evaluation of “smell” has generally been performed using human olfaction. However, since it is necessary to assume that the olfactory sensation varies depending on individual differences in the person (panel) who actually smells the odor and the physical condition of the day, more than a certain number of panels are required to obtain objective results accurately. Ensure sufficient consideration for the environment of the test site. Therefore, the labor and time are enormous. Even if the above points are taken into consideration, it is difficult to always make a definitive judgment based on a certain standard because human olfaction has a characteristic of adapting to “odor”.

  On the other hand, a component analysis method using a gas chromatograph (GC), a gas chromatograph mass spectrometer (GC-MS), or the like is known as an instrumental analysis related to “odor”. However, these component analysis methods recognize odor as a volatile chemical substance, which is effective for purposes such as identifying the causative substance, but it is difficult to correlate with the sensory value based on human olfaction. There are problems such as.

  In order to compensate for the shortcomings of the component analysis method, there is known a smell sniffing-GC-MS device in which a device for sniffing (sniffing port) is attached to a GC-MS device.

FIG. 3 shows a configuration example of a conventional smell sniffing-GC-MS apparatus.
That is, the separation column 303 is installed inside the column oven 302 of the GC 310 controlled to increase the temperature at a predetermined speed, and the analysis sample is introduced from the sample injection / vaporization chamber 301 toward the separation column 303. The introduced sample is separated and developed in the time direction for each component by a combined action such as the temperature gradient of the temperature rise in the column oven 302, the flow rate of the mobile phase gas, and the type and size of the liquid phase of the separation column. Is done. The components separated and expanded in the time direction are introduced into the MS device 306 (for example, a quadrupole mass spectrometer) via the splitter 305, and the mass-to-charge ratio and intensity of molecular ions and their fragment ions are accurately measured. Then, qualitative and quantitative analysis of the components is performed.

  A part of the components separated and developed in the time direction by the separation column 303 is also sent to the sniffing port 309 via the transfer line 308. In the smell sniffing port 309, when the “odor” is detected, the measurer operates the level switch to express the intensity and type of the “odor”.

  Auxiliary gas such as helium gas is supplied from the makeup gas generator 304 to the splitter 305 as an auxiliary means for efficiently sending the “odor” component from the splitter 305 to the MS device 306 and the sniffing port 309.

  Through the above operations, the smell smell-GC-MS measurement combining GC-MS and human olfaction is used to identify the “odor” component and the “odor” intensity and the qualitative / quantitative information of the component. Can be obtained at the same time.

  In addition, since the “odor” analysis depends on the olfactory sense of the measurer, it is necessary to slowly separate and develop the sample with the GC, and the measurement time is as long as 30 to 50 minutes. Meanwhile, the measurer needs to concentrate attention on the olfactory sense, and long-time tension is required. In order to alleviate this burden, Patent Document 1 introduces an invention that notifies that a component appears at the timing when a component peak begins to appear.

JP 2008-170333 A

It is not uncommon for the “scent” analysis to take a long time. In addition, a sample having an irritating odor such as a rotting odor has a problem that the sense of smell is paralyzed and the “odor” component having a low “smell” detection threshold is sniffed. Furthermore, the measurement sample contains harmful compounds, and there is a risk of causing health damage to the measurer.
An object of the present invention is to provide an odor sniffing-GC-MS device that can reduce the burden on a measurer who must maintain concentration over a long period of time and can reduce health damage in view of the above-described points.

The sniff-GC-MS device according to the present invention is
Chromatographic means for separating and developing components in a sample having odor in the time direction;
A mechanism for displaying in real time a chromatogram obtained by the chromatographic means, and a mass analyzing means for taking out a part of the separated and expanded components and sequentially performing mass analysis;
In the sniffer-gas chromatograph mass spectrometer equipped with a transfer line that sends the remainder of the components to the sniffing port,
A database in which mass analysis results and odor information of chromatogram peaks of components separated and developed by the chromatographic means by analyzing known odor components in advance and registered,
Comprising means for selecting component information in the database prior to sample measurement;
Means is provided for extracting the selected component information from the database and notifying the odor information at the holding time position of the chromatogram display mechanism.

  The odor information drawn at the holding time position is preferably a strip-colored display or characters or symbols.

  The selected component information is overlaid on the screen on which the sample chromatogram is displayed. Therefore, based on the relationship between the component information and the chromatogram display position, whether or not the “smell” is registered in the database before sniffing the “smell” of the sample, and if so, what is the component information? It is possible to sniff “smell” after recognizing odor, and avoid measurement errors due to olfactory paralysis due to irritating odor components registered in the database and health damage due to toxic components.

It is a figure which shows the structural example of the smell sniffing-GC-MS apparatus by this invention. It is a figure which shows the example of a monitor display of the smell sniffing-GC-MS apparatus by this invention. (A) is an example in which four types of “scent” information selected in the database is displayed at the holding time position. (B) shows an example in which chromatograms of sample analysis are overdrawn. It is a figure which shows the structural example of the conventional smell sniffing-GC-MS apparatus.

  Embodiments of the present invention will be described below with reference to the drawings.

The basic configuration of the sniff-GC-MS device of the present invention is shown in FIG.
In the sniffer-GC-MS device of the present invention, a known “odor” component is analyzed in advance, and the “compound name”, “mass spectrum”, and retention time of the compound are indexed by a reference substance (n-alkane). A database that stores "holding indicators" such as the "threshold" of the minimum concentration or minimum chromatogram peak value for detecting "odor" quality such as banana scent, rotten "odor", and "odor" 113 is built in a memory in a personal computer (hereinafter referred to as a PC) 107.

  A separation column 103 is installed inside the column oven 102 of the GC 110 that is controlled to rise in temperature at a predetermined speed, and an analysis sample is introduced from the sample injection / vaporization chamber 101 toward the separation column 103. The introduced sample is displayed on the monitor 112 of the PC 107 as a chromatogram separated and developed in the time direction for each component.

  The components separated and expanded in the time direction are supplied from a makeup gas generator 104 to an auxiliary gas such as helium gas to a splitter 105 and introduced into an MS device 106 (for example, a quadrupole mass spectrometer). Is sent to the transfer line 108, reaches the smell sniffing port 109, and the measurer sniffs “smell” and inputs “smell” information.

  Components sent to the MS device 106 and the GC 110 are analyzed by MS and GC, and component information is displayed on the monitor 112 of the PC 107.

  In the smell sniffing-GC-MS apparatus having the above-described configuration, at the start of sample measurement, the operator, from the components in the database, is expected to cause a component that is expected to be included in the sample or an olfaction or health hazard. Select ingredients. The selected component information is extracted from the database, and “odor” information is displayed at the holding time position of the monitor 112 of the PC 107. FIG. 2A shows an example of the display.

  In this example, four types of “scents” (limonene, octanol, skatole, menthol) are selected, and a strip at each holding time position (7.51 minutes, 11.34 minutes, 13.84 minutes, 16.34 minutes). -Shaped fills appear, and the selected "odor" information 201-204 is displayed therein.

  Next, the sample is introduced from the sample injection / vaporization chamber 101 toward the separation column 103. The introduced sample is overlaid on the monitor 112 of the PC 107 as a chromatogram separated and developed in the time direction for each component. FIG. 2B shows an example. A chromatogram 205 of about 10 minutes is drawn. In this example, the odor of limonene has already ended, the odor of soapy octanol after 1.3 minutes, the stool of fecal odor after 3.8 minutes, and the mint smell of mint odor after 6.3 minutes. Can be expected to reach the smell port.

  As described above, the operator smells “odor” next from the display positional relationship between the “odor” information expected to be included in the sample and the chromatogram in which the “odor” component of the sample is separated and developed in the time direction. Information can be expected. Therefore, measurement errors due to olfactory paralysis due to stimulating odor components registered in the database and health damage due to toxic components can be avoided.

  As a modified example of the first embodiment, the strip-shaped filling displayed on the PC monitor may express the quality of “odor” in red if it causes health damage, for example, yellow if it is an irritating odor. it can.

  As a modification of the first embodiment, the “smell” information displayed on the PC monitor displays only the reference number at the holding time position, the detailed information is displayed in a separate window, and the detailed information is referred to from the reference number. You can also.

  As a modification of the first embodiment, it is possible to separately provide a PC monitor that displays the same content as the PC 107 in the field of view of the measurer near the smell sniffing port.

101 Sample Injection / Vaporization Chamber 102 Column Oven 103 Separation Column 104 Makeup Gas Generator 105 Splitter 106 MS Device 107 Personal Computer (PC)
108 Transfer line 109 Smell port 110 GC
112 Monitor 113 Database 201 Selected “odor” information 1
202 Selected “scent” information 2
203 Selected "scent" information 3
204 Selected “scent” information 4
205 Chromatogram 301 Sample Injection / Vaporization Chamber 302 Column Oven 303 Separation Column 304 Makeup Gas Generator 305 Splitter 306 MS Device 308 Transfer Line 309 Sniff Port 310 GC

Claims (2)

Chromatographic means for separating and developing components in a sample having odor in the time direction;
A mechanism for displaying in real time the chromatogram obtained by the chromatographic means;
A mass analyzing means for taking out a part of the separated and expanded components and sequentially performing mass analysis;
In the sniffer-gas chromatograph mass spectrometer equipped with a transfer line that sends the remainder of the components to the sniffing port,
A database in which mass analysis results and odor information of chromatogram peaks of components separated and developed by the chromatographic means by analyzing known odor components in advance and registered,
Comprising means for selecting component information in the database prior to sample measurement;
A smell sniffer-gas chromatograph mass spectrometer characterized by comprising means for extracting the selected component information from the database and notifying the smell information at the holding time position of the chromatogram display mechanism.   2. The smell sniffing-gas chromatograph mass spectrometer according to claim 1, wherein the smell information notified to the holding time position is a strip-colored display or characters or symbols.