JPH1010111A - Breath analyzer - Google Patents

Abstract

(57) [Summary] [PROBLEMS] To enable analysis of low-concentration components such as pentane which are only slightly contained in breath. A breath analyzer (10) according to the present invention includes a separation column (12) for passing a breath sample (A) and separating components contained in the breath sample (A), and a collection tube (14) in which the breath sample (A) is adsorbed. A concentrated sample introduction unit 16 for desorbing the breath sample A adsorbed in the collection tube 14, and a concentrated sample introduction unit 16
A carrier gas control unit 18 having a function of passing the breath sample A desorbed in step 2 through the separation column 12 with the carrier gas C and a function of separately passing the carrier gas C through the concentrated sample introduction unit 16 and the separation column 12; 1
And a detector 20 for detecting the components separated by the two.

Description

DETAILED DESCRIPTION OF THE INVENTION

[0001]

BACKGROUND OF THE INVENTION 1. Field of the Invention The present invention relates to a breath analyzer for analyzing components contained in breath using gas chromatography in the medical field, the health industry, the control of drunk driving, the investigation of narcotics, and the like.

[0002]

2. Description of the Related Art Conventionally, as described in, for example, JP-A-6-58919, a breath analyzer for collecting and analyzing the breath of a subject has been developed. Breath analyzers are, for example, breath analysis for clinical tests in the medical field and monitoring of patient condition, measurement of work environment and indoor environment in the industrial field, drunk driving control and drug control in the police field, and firefighting field. It is used in a wide range of fields such as fire cause investigation and health care in the health industry field.

[0003] This breath analyzer uses gas chromatography. The breath analyzer is attached to the main body of the breath analyzer and has an outer peripheral portion covered with a heater. Two carrier gas flow paths each connected via a four-way electromagnetic valve, an air cylinder connected to the four-way electromagnetic valve, and a sample measuring section provided by partitioning a part of each carrier gas flow path; It has.

[0004] On the downstream side of each sample measuring section, a breathing introduction pump (suction pump) connected via a three-way electromagnetic valve and an exhaust pipe is provided. In addition, each of the three-way solenoid valves is provided with two separation columns and the like connected in parallel and independently of each other.

[0005] In the case of collecting and analyzing exhaled breath from a subject, when the subject exhales into the exhalation collection tube, the exhaled breath is discharged into the exhalation collection tube by the exhalation introduction pump. While being discharged to the outside of the device, a part of the breath is filled in each sample measuring section as a breath sample. Next, when the carrier gas is sent from the air cylinder to each sample measuring section, after the breath sample filled in each measuring section is sent to each separation column, each breath sample is separated by a difference in the retention time of each component gas. Separated. Thereafter, the breath analysis is performed by a predetermined calculation process.

[0006]

For example, in diabetes, the perspiration concentration of pentane increases due to lipid peroxidation, and the concentration value is at most on the order of pg / mL. However, in the conventional breath analyzer, for example, since the limit of the component that can be analyzed is, for example, on the order of ng / mL, pg / mL of pentane or the like is used.
There is a disadvantage that low-order components of the order cannot be analyzed.

[0007]

SUMMARY OF THE INVENTION Therefore, a main object of the present invention is to provide a breath analyzer which can solve the disadvantages of the prior art and can analyze even low-concentration components such as pentane which are slightly contained in breath. It is in.

[0008]

A breath analyzer according to the present invention comprises a separation column for passing a breath sample to separate components contained in the breath sample, and a collection tube for adsorbing the breath sample therein. A concentrated sample introduction unit for desorbing the breath sample adsorbed in the collection tube, a function of passing the breath sample desorbed in the concentrated sample introduction unit through the separation column by a carrier gas, and the concentrated sample introduction unit And a carrier gas control unit having a function of separately passing a carrier gas through the separation column, and a detector for detecting a component separated by the separation column.

The breath sample concentrated and collected in the collection tube is desorbed at the concentrated sample introduction part, and passes through the separation column together with the carrier gas. The concentration of the breath sample with respect to the carrier gas is much higher than when the non-concentrated breath sample is flowed together with the carrier gas. That is, the detector can obtain a detection value with a high peak. Therefore, even low-concentration components that are slightly contained in the breath can be sufficiently analyzed. Moreover, by separately passing the carrier gas through the concentrated sample introduction section and the separation column, the carrier gas is allowed to flow through the separation column to continue the analysis, while the collection tube is detached or the carrier gas is allowed to flow through the collection tube. To clean and regenerate the collection tube.

[0010]

DETAILED DESCRIPTION OF THE PREFERRED EMBODIMENTS FIGS. 1 to 3 are configuration diagrams showing an embodiment of a breath analyzer according to the present invention. FIGS. 4 to 6 are schematic cross-sectional views showing the flow path switching valve in the breath analyzer of FIGS. FIGS. 1 and 4 show the state when the collection tube is attached or detached or on standby, FIGS. 2 and 5 show the state when the breath sample is detached, and FIGS. 3 and 6 show the continuation of the analysis and the washing / regeneration of the collection tube. Indicates time. FIG. 7 is a cross-sectional configuration diagram illustrating an example of the breath concentration and collection device. Hereinafter, description will be made based on these drawings.

A breath analyzer 10 according to the present invention includes a separation column 12 for passing a breath sample A to separate components contained in the breath sample A, a collection tube 14 having the breath sample A adsorbed therein, A concentrated sample introduction unit 16 for desorbing the breath sample A adsorbed in the collection tube 14, a function for passing the breath sample A desorbed in the concentrated sample introduction unit 16 to the separation column 12 by the carrier gas C, and a concentration. A carrier gas control unit 18 having a function of separately passing a carrier gas C through the sample introduction unit 16 and the separation column 12;
And a detector 20 for detecting the components separated by the above.

The separation column 12 is, for example, a capillary column or a packed column. Concentrated sample introduction unit 16
Supports the collection tube 14 and heats the collection tube 14 with a heater (not shown) to desorb the breath sample A adsorbed in the collection tube 14. The detector 20 may detect any of mass, heat conduction, ionic current, and the like.

The carrier gas control section 18 includes a carrier gas flow path 181 for guiding the carrier gas C via the concentrated sample introduction section 16, a carrier gas flow path 182 for directly leading the carrier gas C, an exhaust pipe 183, Flow path switching valve 18
And control means 185 for controlling the flow path switching valve 184
And An electromagnetic valve 187 is provided in the carrier gas channel 181, and an electromagnetic valve 188 is provided in the carrier gas channel 182.
2 is a mass flow controller 189 for keeping the flow rate constant.
Is provided. The carrier gas flow paths 181 and 182 and other piping are preferably those whose inner walls are inactivated by a quartz coating or the like, and the length thereof is preferably as short as possible. In particular, the path leading to the concentrated sample introduction section 16, the carrier gas flow path 181, and the separation column 12 is made as short as possible.

The flow path switching valve 184 includes an electromagnetic valve 191 for connecting or shutting off the carrier gas flow path 181 and the separation column 12, an electromagnetic valve 192 for connecting or shutting off the carrier gas flow path 181 and the exhaust pipe 183, Carrier gas channel 1
Solenoid valve 19 for connecting or disconnecting 82 from separation column 12
3 is provided. Solenoid valves 187, 188, 191-1
Each of the control valves 93 is a check valve type, and is controlled to be energized by a control unit 185. The solenoid valves 187,.
It is preferable that the gas contact portion is deactivated by a quartz coating or the like. The solenoid valves 191 to 193 may be mechanical check valves.

A gas cylinder 221 filled with a carrier gas C is provided in the carrier gas control section 18 by a pressure reducing valve 222.
And a manual valve 223. As the carrier gas C, air, hydrogen, nitrogen, helium, argon or the like is generally used. Further, the carrier gas control unit 18 includes a flow path switching valve 184 and electromagnetic valves 187, 1
Control means 185 is provided for controlling the energization of the solenoids 88 and the like. The control means 185 may be of any type, including a manual switch, a relay and a timer, and a microcomputer and its program. The flow path switching valve 184, the separation column 12, the detector 20, and the piping around them are housed in a thermostat (not shown) kept at a constant temperature of 100 ° C., for example.

Next, the operation of the breath analyzer 10 will be described.

First, the breath sample A is adsorbed on the collection tube 14 using the breath concentration / collection device 80 shown in FIG. The exhaled breath collection device 80 includes a Tedlar bag 82 filled with the exhaled air A ′, a collection tube 14 communicating with the Tedlar bag 82, and an exhaled air A ′ in the Tedlar bag 82.
A pump 84 for suctioning the air through the collecting tube 14, an integrating flow meter 86 for measuring the integrated flow rate f of the exhalation A 'passing through the collection tube 14, a pressure gauge 88 for measuring the pressure p of the exhalation A' in the Tedlar bag 82, and a pressure gauge a main control unit 90 that the pressure p of the measured expiratory a 'stops the pump 84 when it becomes less than a predetermined value p _F 88, an incubator 92 for a constant temperature T of the collecting tube 14, capturing A water absorption filter 94 is provided in the flow path of the exhalation A ′ between the collecting pipe 14 and the pump 84. Tedlar bag 82, T-tube 881 of pressure gauge 88,
The collection tube 14, the water absorption filter 94, the pump 84, and the integrating flow meter 86 are connected by flexible tubes 95a to 95e, respectively.

The collection tube 14 is filled with an adsorbent 141 for adsorbing the breath sample A. Tedlar bag 82
Has an exhalation discharge port 821 and an exhalation blowout port 822. Although not shown, the exhalation discharge port 821 and the exhalation blow port 822 are provided with stop valves that can be manually opened and closed. In advance, the subject attaches the disposable mouthpiece 823 to the breath inlet 822 and
3 and the exhalation A ′ is blown into the Tedlar bag 82. The integrating flow meter 86 is a general gas flow meter such as a mass flow meter. The pressure gauge 88 uses, for example, a piezoelectric effect that generates a voltage when a pressure is applied to a piezoelectric element, and outputs an electric signal corresponding to the pressure p of the exhalation A ′ to the main control unit 90. The main control unit 90 includes, for example, a microcomputer including a CPU, a ROM, a RAM, an input / output interface, and the like, and a computer program stored in the ROM or the like. The operation of the main control unit 90, drives the pump 84 with stops when the pressure p of exhalation A 'output from the pressure gauge 88 becomes equal to or less than a predetermined value p _F, buzzer for informing not shown, the lamp It is programmed to be. According to experiments, the pressure p during suction is, for example, -0.05 kgf / cm ² ,
The pressure p at the end of suction (that is, the constant value p _F ) is, for example, −0.3 to −0.4 kgf / cm ² . The thermostat 92 includes a heating / cooling unit 96 and a temperature control unit 97. The heating and cooling unit 96 can be divided into an upper side 98 and a lower side 99, and the upper side 98 and the lower side 99 sandwich the collection tube 14. Therefore, the collection tube 14 is connected to the heating / cooling unit 96.
Can be easily attached and detached. The upper side 98 is composed of a heat insulating material 981, a heat transfer material 982, and the like. The lower side 99 is a heat insulating material 9
91, a heat transfer material 992, a Peltier element 993, a radiation fin 994, and the like. The heat transfer members 982, 992 and the radiation fins 994 are made of aluminum. A thermocouple 971 is embedded inside the heat transfer material 992. The thermocouple 971 outputs a voltage corresponding to the temperature T of the heat transfer material 992, that is, the temperature of the collection tube 14, to the temperature control unit 97. The temperature control unit 97 includes, for example, a microcomputer including a CPU, a ROM, a RAM, an input / output interface, and the like.
It is composed of a computer program for temperature control stored in the OM or the like, and a DC voltage power supply. Operation of the temperature control unit 97, as the temperature T of the collecting tube 14, which is outputted from the thermocouple 971 is a constant value T _C, in which the Peltier element 993 for controlling energization. When the fixed value T _C is equal to or higher than room temperature, a simple electric heater or the like may be used instead of the Peltier element 993. Inside the moisture absorption filter 94, a hygroscopic material 941 such as silica gel, calcium carbonate or the like is provided.
Is filled.

When the pump 86 operates, the exhalation A ′ is sucked from the Tedlar bag 82 through the collection tube 14. Thereby, the exhalation component A is concentrated and collected by the adsorbent 141 of the collection tube 14. At this time, the pressure p during suction is measured by the pressure gauge 88, and the integrated flow rate f is measured by the integrated flow meter 86. If Tedlar bag 82 is emptied, the pressure p reaches a predetermined value p _F, the main control unit 90 is a pump 8
4 is stopped. The integrated flow rate f at the end of the suction is output from the integrated flow meter 86 to the main control unit 90.
The amount of expiration A 'concentrated in the water is also known.

Subsequently, in the state shown in FIGS. 1 and 4, the collection tube 14 is attached to the concentrated sample introduction section 16. At this time, the control means 185 controls the solenoid valves 187, 19
1, 192 is closed, and the solenoid valves 188, 193 are open. Therefore, the carrier gas C flows in the order of the carrier gas flow path 182 → the separation column 12 → the detector 20 → the discharge, purging the separation column 12 and the detector 20.
In addition, the display means (not shown) displays, for example, “under preparation” based on the output signal from the control means 185.

Subsequently, in the state shown in FIGS. 2 and 5, the collection tube 14 is heated at, for example, 250 ° C. for 5 minutes. Under this condition, most of the exhalation component A adsorbed on the collection tube 14 is desorbed. At this time, the solenoid valves 188, 192 and 193 are closed by the control means 185, and the solenoid valve 18 is closed.
7,191 is open. Accordingly, the carrier gas C flows in the order of the carrier gas flow path 181 (collection tube 14) → separation column 12 → detector 20 → discharge.
The breath sample A desorbed in 4 is sent to the separation column 12. Each component contained in the breath sample A is separated from the separation column 12
, The detector 2 has a time difference
0 is detected. The detector 20 performs qualitative analysis based on the volume (retention capacity) or the time (retention time) of the carrier gas C from the time when the breath sample A is injected until the separation zone of each component appears, and the peak area or peak height is determined. Thus, a quantitative analysis is performed. According to the breath analyzer 10, since the breath sample A concentrated by the concentrated sample introduction unit 16 is used, it is possible to sufficiently analyze even low-concentration components such as pentane in which only pg / mL is contained in the breath. Can be. In addition, the display means (not shown) displays, for example, "during detachment" and "during analysis" based on the output signal from the control means 185.

Subsequently, in the state shown in FIGS. 3 and 6, the analysis is continued and the collection tube 14 is washed and regenerated. At this time, the electromagnetic valve 191 is closed by the control means 185,
The solenoid valves 187, 188, 192, 193 are open. Therefore, the carrier gas C flows in the order of the carrier gas flow path 182 → the separation column 12 → the detector 20 → discharge, and the flow of the carrier gas flow path 181 (the collection pipe 14) → the discharge pipe 183 → discharge. The former flow of the carrier gas C is for continuing the analysis. This is because it takes about one hour for all of the exhalation component A to pass through the separation column 12. The latter flow of the carrier gas C is for cleaning and regeneration of the collection tube 14. Collection tube 14
At the time of washing and regenerating, the collection tube 14 is heated to, for example, 300 ° C. In this way, during the continuation of the analysis,
Since regeneration can be performed, continuation of analysis and collection tube 14 can be performed.
The analysis time can be shortened or the equipment can be simplified as compared with the case where the washing and regeneration are performed separately. For example, 1
If it takes 5 minutes to wash and regenerate, about 5 minutes
Minutes can be reduced. In the display means (not shown),
For example, “during analysis” and “during playback” are displayed based on the output signal from the control unit 185.

The above embodiment is, of course, merely an example, and does not limit the present invention. For example,
The flow path switching valve 184 may be a rotary valve. The function of controlling the concentrated sample introduction unit 16 and the detector 20 and performing data processing may be added to the control unit 185 so that the breath analyzer 10 may be completely automated. The control means 185 may be provided with a manual mode for selecting whether or not to regenerate the collection tube 14.

[0024]

According to the breath analyzer according to the present invention, the breath sample concentrated and collected in the collection tube is desorbed at the concentrated sample introduction section, and the breath sample is passed through the separation column by the carrier gas. Therefore, even low-concentration components such as pentane, which are contained only a little in the breath, can be sufficiently analyzed.

In addition, by separately passing the carrier gas through the concentrated sample introduction section and the separation column, the carrier gas is allowed to flow through the separation column to continue the analysis, and the collection tube can be attached and detached or the carrier tube can be inserted into the collection tube. It is possible to wash and regenerate the collection tube by flowing gas. Therefore, as compared with the case where the cleaning / regeneration of the collection tube is performed by the device dedicated to cleaning / regeneration, the device dedicated to cleaning / regeneration is not required, so that the equipment can be simplified, and the collection tube can be transferred between the devices. Since it becomes unnecessary, the work of attaching and detaching the collection tube can be reduced. In addition, compared to the case where a single breath analyzer performs analysis of a breath sample and cleaning / regeneration of the collection tube at different times, analysis of the breath sample and cleaning / collection of the collection tube are performed.
Since the reproduction can be performed at the same time, the analysis time can be reduced.

[Brief description of the drawings]

FIG. 1 is a configuration diagram showing one embodiment of a breath analyzer according to the present invention, showing a state when a collection tube is attached or detached or a standby state.

FIG. 2 is a configuration diagram showing an embodiment of a breath analyzer according to the present invention, showing a state in which a breath sample is detached.

FIG. 3 is a configuration diagram showing an embodiment of a breath analyzer according to the present invention, showing continuation of analysis and washing / regeneration of the collection tube.

FIG. 4 is a schematic sectional view of a flow path switching valve in a state of the breath analyzer of FIG. 1;

FIG. 5 is a schematic sectional view of a flow path switching valve in a state of the breath analyzer of FIG. 2;

FIG. 6 is a schematic sectional view of a flow path switching valve in a state of the breath analyzer of FIG. 3;

FIG. 7 is a cross-sectional configuration diagram illustrating an example of a breath concentration / collection device.

[Explanation of symbols]

 DESCRIPTION OF SYMBOLS 10 Breath analyzer 12 Separation column 14 Collection tube 16 Concentrated sample introduction part 18 Carrier gas control part 20 Detector 181 First carrier gas flow path 182 Second carrier gas flow path 183 Exhaust pipe 184 Flow path switching valve 185 Control Means 191, 192, 193 Solenoid valve A Breath sample C Carrier gas

Claims (2)

[Claims] 1. A separation column through which a breath sample is passed to separate components contained in the breath sample, a collection tube having the breath sample adsorbed therein, and a breath sample adsorbed in the collection tube. A concentrated sample introduction unit to be desorbed, a function of passing the breath sample desorbed in the concentrated sample introduction unit through the separation column by a carrier gas, and a function of separately passing a carrier gas through the concentrated sample introduction unit and the separation column An exhalation analyzer comprising: a carrier gas control unit having: and a detector for detecting components separated by the separation column. 2. The carrier gas control section includes: a first carrier gas flow path that guides the carrier gas through the concentrated sample introduction section; and a second carrier gas flow path that directly guides the carrier gas. An exhaust pipe, a flow path switching valve, and control means for controlling the flow path switching valve, wherein the flow path switching valve is configured to connect or shut off the first carrier gas flow path and the separation column. A valve, an electromagnetic valve for connecting or shutting off the first carrier gas flow path and the exhaust pipe, and an electromagnetic valve for connecting or shutting off the second carrier gas flow path and the separation column, The breath analyzer according to claim 1.