WO2012033455A1 - Échantillonneur d'air pour l'air expiré utilisant un prélèvement de composés et de gaz sur un dispositif adsorbant approprié - Google Patents

Échantillonneur d'air pour l'air expiré utilisant un prélèvement de composés et de gaz sur un dispositif adsorbant approprié Download PDF

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Publication number
WO2012033455A1
WO2012033455A1 PCT/SE2011/051082 SE2011051082W WO2012033455A1 WO 2012033455 A1 WO2012033455 A1 WO 2012033455A1 SE 2011051082 W SE2011051082 W SE 2011051082W WO 2012033455 A1 WO2012033455 A1 WO 2012033455A1
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WO
WIPO (PCT)
Prior art keywords
fibre
inlet
spme
sample air
mode
Prior art date
Application number
PCT/SE2011/051082
Other languages
English (en)
Inventor
Lennart Olsson
Hans Verner Lagesson
Original Assignee
Chromalytica Ab
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Chromalytica Ab filed Critical Chromalytica Ab
Publication of WO2012033455A1 publication Critical patent/WO2012033455A1/fr

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Classifications

    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N1/00—Sampling; Preparing specimens for investigation
    • G01N1/02—Devices for withdrawing samples
    • G01N1/22—Devices for withdrawing samples in the gaseous state
    • G01N1/2202—Devices for withdrawing samples in the gaseous state involving separation of sample components during sampling
    • G01N1/2214—Devices for withdrawing samples in the gaseous state involving separation of sample components during sampling by sorption
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N33/00—Investigating or analysing materials by specific methods not covered by groups G01N1/00 - G01N31/00
    • G01N33/48—Biological material, e.g. blood, urine; Haemocytometers
    • G01N33/483—Physical analysis of biological material
    • G01N33/497—Physical analysis of biological material of gaseous biological material, e.g. breath
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N1/00—Sampling; Preparing specimens for investigation
    • G01N1/02—Devices for withdrawing samples
    • G01N1/22—Devices for withdrawing samples in the gaseous state
    • G01N1/2273—Atmospheric sampling
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N1/00—Sampling; Preparing specimens for investigation
    • G01N1/02—Devices for withdrawing samples
    • G01N1/22—Devices for withdrawing samples in the gaseous state
    • G01N2001/2244—Exhaled gas, e.g. alcohol detecting
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N1/00—Sampling; Preparing specimens for investigation
    • G01N1/02—Devices for withdrawing samples
    • G01N1/22—Devices for withdrawing samples in the gaseous state
    • G01N2001/2285—Details of probe structures

Definitions

  • the present invention concerns air sampling and collection of volatile compounds and gases at low concentrations in exhaled breath and other gases.
  • the compounds found in exhaled breath are used as biomarkers of diseases like lung cancer, asthma and diabetes.
  • the presence of compounds in exhaled breath can also be used for evaluation of for example
  • the basic technology is known and usually involves exhaled breath collected in a Tedlar or Mylar bag or a plastic or glass cylinder.
  • a solid phase micro extraction (SPME) fiber is inserted, through a septum, into the Tedlar bag or glass bottle for at least 30 min and typically several hours at room temperature to extract the volatile compounds (VOC ' s).
  • SPME is an attractive solvent free alternative, which combines sampling and pre concentration in one step.
  • the SPME technology is also inexpensive and has high time efficiency and is used for both air and liquids.
  • the drawbacks for a conventional static air sampling are long sampling time, low recovery and unsatisfied reproducibility.
  • the object of the present invention is to eliminate the drawbacks mentioned above.
  • the invention relates to physical, mechanical and software control solutions.
  • the invention solves major problems and shortcomings with present technology, is very versatile and can be used for various applications.
  • One particular use is for detection of metabolic or other substances emanating from living cells, tissues and in particular that can be found in exhaled air, saliva, sweat, blood and urine from humans, animals, organisms and plants etc. for detection of various deceases and metabolic activities like stress.
  • Substances can be such as nitrogen oxide, urea, acetone, isoprene, carbon disulfide coming from diseases like cancer, gastric ulcers, asthma, diabetes, psychiatric disorders, drug abuse, stress conditions and intoxications, etc.
  • the present invention is based on a dynamic collection from a constant exhaled air flow. This implies that the exhaled breath air is passing the adsorption fibre at a relatively high speed. In this mode the thickness of the static boundary air layer surrounding the SPME fibre is reduced and the sorption rate is considerably increased. This in turn gives a considerably shorter sampling time, a much higher recovery and better reproducibility.
  • One or a plurality of SPME fibres can be used.
  • Exhaled breath is, by nature, a pulsating flow. Moreover there is a need for analysing mixed expiratory air as well as exhaled air consisting mainly of the alveolar portion of the air.
  • the alveolar air is pushed out actively by the test subject.
  • the present invention solves these situation in an effective and yet simple way.
  • the biomarkers for various diseases are most often present in the exhaled breath at very low concentrations. This situation implies that risks for adsorption on and diffusion into materials in contact with the exhaled breath sample must be minimized. This is taken into consideration in the present invention.
  • the chemical analysis of the compounds trapped on to the SPME fibre are preferably carried out by gas chromatography hyphenated with ultraviolet light absorption (GC-UV) but the method of analysis could also be gas chromatography linked to mass spectroscopy (GC-MS) or any other method of analyze.
  • a dynamic sample air flow of the exhaled breath is created along with the SPME fibre.
  • a suitable, relatively high flow rate is obtained by leading the air through a narrow bore glass tubing surrounding the SPME fibre.
  • the flow arrangement comprises a T formed glass tubing construction.
  • a first opening has a septum for the penetration of the SPME needle.
  • a second opening is for the inlet of the exhaled breath air flow.
  • a third opening is connected to a pump which can draw a variable air flow of 1 - 100 ml/min giving an air flow rate along with the fibre of 1 - 100 cm/sec.
  • a third aspect of the invention there are two modes of exhaled breath sampling.
  • the first mode (A) there is a requirement that the test person is able to participate actively in the sampling procedure.
  • the second mode (B) implies that the mixed exhaled breath is drawn directly to the adsorbent layer of the fibre. In this mode there is no need for the test person to participate actively in the sampling process.
  • a temporary exhaled breath air compartment consisting of preferably a cylinder 20 - 30 mm in diameter and 200 - 300 mm long.
  • the glass or plastic cylinder is internally Al coated or silanized in order to minimize losses due to adsorption or diffusion into the walls of the compartment.
  • the exhaled breath compartment has an inlet for the exhaled breath coming from the test person and an outlet going to a three way valve which in turn is leading to the inlet for the exposure to the SPME fibre.
  • the three way valve In the A inlet mode the three way valve is open to the compartment and in the B mode the three way valve is open for the B mode flow.
  • a fifth aspect of invention it can be used in any sampling of unidentified gas and/or mixed gases that have to be identified and quantified.
  • Fig. 1 shows the direction of sample air along with the SPME fibre.
  • Fig. 2 shows the flow arrangement in the T shaped glass tubing device comprising (1 ) Inlet of air sample flow (2) septum for SPME needle insertion (3) SPME needle (4) coated adsorption fibre (5) outlet leading to a pump able to giving variable flow rates.
  • Fig. 3 shows the whole set up of the exhaled breath sampling device with the mode A and mode B combined exhaled breath inlets in one unit.
  • Fig. 4 shows a cross section of gas flow perpendicular to the SPME coated adsorption fibre (5) and with gas flow (9)
  • the invention relates to a method of considerable improvement of the versatility, speed, recovery and reproducibility for sampling of volatile compounds and gases in exhaled breath.
  • the SPME technology is employed whereby the compounds of interest are trapped and adsorbed on a SPME fibre with various coatings treatments on the fibre.
  • a plurality of fibres are used. Different fibres can be used in parallel for improved simultaneous or sequential adsorbtion.
  • the present invention uses a dynamic constant flow air sampling. The optimum air flow rate depends to some extent on the volatility of the compounds to be determined.
  • the qualitative and quantitative analysis of the compounds adsorbed on the SPME fibre are preferably analysed with gas chromatography hyphenated with UV spectrophotometry (GC-UV) but gas chromatography hyphenated with mass spectroscopy or other detector principles can also be used.
  • GC-UV UV spectrophotometry
  • Fig. 1 shows the direction of exhaled breath air flow along with the SPME fibre.
  • Fig. 2 shows the exhaled breath air flow arrangement within a T shaped glass device with internal diameter of 1 - 2 mm. The narrow diameter of the tubing has the function of giving a high air flow speed at relatively low flow rates.
  • the exhaled air flow inlet is at (1 ) and the septum (2) serves as a gas tight device for the insertion of the SPME needle (3).
  • the position of the SPME fibre (4) is in the part of the T as shown by the figure.
  • the creation of the flow is made by a pump (not shown) connected at (5) and drawing the air sample through the system at preset various constant air flows.
  • the pump is preferably battery driven.
  • Fig. 3 shows the whole combined invention device comprising the flow arrangement shown in Fig. 2 and a temporary hold (6) for up for exhaled breath air.
  • This compartment consists of a tubing 20 - 30 mm in diameter and having a length of 200 - 300 mm. It has a wall thickness of 1 - 2 mm and is preferably made of a plastic or glass material.
  • the inner part of the wall has an Al coating or a silanized preventive layer.
  • the temporary hold up cylinder is thermally isolated to some extent in order to minimize condensation of the water vapour content in the exhaled breath.
  • the air inlet occurs as shown and the outlet is at (8).
  • the temporary hold up compartment is in connection with a three way valve (7) and at the A mode air sampling the air is drawn up to the SPME fibre by means of a pump.
  • a compartement (6) for temporary exhaled breath air is connected to the three way valve (7). Exhaled breath waste may exit at the outlet (8).
  • valve position In the B mode sampling the valve position is turned 90 ° counter clockwise and the sampling air is drawn directly from the position of sampling (B mode inlet) up to the SPME fibre.
  • Fig. 4 shows a cross section of gas flow perpendicular to the SPME coated adsorption fibre (5) and with gas flow (9)

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  • Life Sciences & Earth Sciences (AREA)
  • Health & Medical Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Chemical & Material Sciences (AREA)
  • Molecular Biology (AREA)
  • Physics & Mathematics (AREA)
  • Biomedical Technology (AREA)
  • General Physics & Mathematics (AREA)
  • Analytical Chemistry (AREA)
  • Biochemistry (AREA)
  • General Health & Medical Sciences (AREA)
  • Immunology (AREA)
  • Pathology (AREA)
  • Urology & Nephrology (AREA)
  • Hematology (AREA)
  • Food Science & Technology (AREA)
  • Medicinal Chemistry (AREA)
  • Biophysics (AREA)
  • Sampling And Sample Adjustment (AREA)
  • Investigating Or Analysing Biological Materials (AREA)

Abstract

L'invention concerne un procédé et une solution permettant d'échantillonner et de prélever des composés chimiques présents dans l'air expiré, dans l'atmosphère ou dans d'autres gaz. Ce procédé et cette solution reposent sur l'échantillonnage dynamique d'un écoulement d'air/gaz sur une fibre de microextraction en phase solide (SPME). Selon un mode A, l'échantillon d'air expiré est envoyé par soufflage dans un compartiment de retenue provisoire avant d'être aspiré, pompé par la fibre d'adsorption SPME. Selon un mode B, l'échantillon d'air est aspiré par la pompe pour être introduit directement dans la fibre SPME.
PCT/SE2011/051082 2010-09-09 2011-09-07 Échantillonneur d'air pour l'air expiré utilisant un prélèvement de composés et de gaz sur un dispositif adsorbant approprié WO2012033455A1 (fr)

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
US38141510P 2010-09-09 2010-09-09
US61/381,415 2010-09-09

Publications (1)

Publication Number Publication Date
WO2012033455A1 true WO2012033455A1 (fr) 2012-03-15

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Cited By (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN104165785A (zh) * 2014-07-28 2014-11-26 武汉碧海云天科技股份有限公司 一种智能恒流低流量气体采集检测装置与方法
US10052045B2 (en) 2012-12-21 2018-08-21 Colgate-Palmolive Company Method for testing oral malodor
WO2018192447A1 (fr) * 2017-04-17 2018-10-25 武汉大学 Procédé d'injection d'échantillon d'enrichissement de micro-colonne
CN110715832A (zh) * 2019-10-22 2020-01-21 好维股份有限公司 用于口气检测的主动式采样器及与气相色谱联用分析方法
CN112763611A (zh) * 2020-12-28 2021-05-07 中山大学 一种准确测定环境空气中半挥发性有机物浓度的装置及方法
WO2022055425A1 (fr) * 2020-09-08 2022-03-17 National University Of Singapore Appareil de collecte d'haleine expirée

Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
FR2873812A1 (fr) * 2004-07-28 2006-02-03 Air Liquide Dispositif de prelevement de composes volatils
US20060260419A1 (en) * 2005-05-18 2006-11-23 The Regents Of The University Of California Offline solid phase microextraction sampling system

Patent Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
FR2873812A1 (fr) * 2004-07-28 2006-02-03 Air Liquide Dispositif de prelevement de composes volatils
US20060260419A1 (en) * 2005-05-18 2006-11-23 The Regents Of The University Of California Offline solid phase microextraction sampling system

Non-Patent Citations (3)

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Title
CHEN Y ET AL: "CALIBRATION FOR ON-SITE ANALYSIS OF HYDROCARBONS IN AQUEOUS AND GASEOUS SAMPLES USING SOLID-PHASE MICROEXTRACTION", ANALYTICAL CHEMISTRY, AMERICAN CHEMICAL SOCIETY, US, vol. 75, no. 23, 1 December 2003 (2003-12-01), pages 6485 - 6493, XP001047348, ISSN: 0003-2700, DOI: 10.1021/AC0349328 *
KOZIEL J A ET AL: "System for the generation of standard gas mixtures of volatile and semi-volatile organic compounds for calibrations of solid-phase microextraction and other sampling devices", JOURNAL OF CHROMATOGRAPHY, ELSEVIER SCIENCE PUBLISHERS B.V, NL, vol. 1025, no. 1, 30 January 2004 (2004-01-30), pages 3 - 9, XP004480714, ISSN: 0021-9673, DOI: 10.1016/J.CHROMA.2003.10.079 *
XIONG G ET AL: "Air sampling of aromatic hydrocarbons in the presence of ozone by solid-phase microextraction", JOURNAL OF CHROMATOGRAPHY, ELSEVIER SCIENCE PUBLISHERS B.V, NL, vol. 1025, no. 1, 30 January 2004 (2004-01-30), pages 57 - 62, XP004480721, ISSN: 0021-9673, DOI: 10.1016/J.CHROMA.2003.10.078 *

Cited By (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US10052045B2 (en) 2012-12-21 2018-08-21 Colgate-Palmolive Company Method for testing oral malodor
CN104165785A (zh) * 2014-07-28 2014-11-26 武汉碧海云天科技股份有限公司 一种智能恒流低流量气体采集检测装置与方法
WO2018192447A1 (fr) * 2017-04-17 2018-10-25 武汉大学 Procédé d'injection d'échantillon d'enrichissement de micro-colonne
US11287401B2 (en) 2017-04-17 2022-03-29 Wuhan Spenrich Technologies Co., Ltd Sample pretreatment method of microextraction tube injection
CN110715832A (zh) * 2019-10-22 2020-01-21 好维股份有限公司 用于口气检测的主动式采样器及与气相色谱联用分析方法
WO2022055425A1 (fr) * 2020-09-08 2022-03-17 National University Of Singapore Appareil de collecte d'haleine expirée
CN112763611A (zh) * 2020-12-28 2021-05-07 中山大学 一种准确测定环境空气中半挥发性有机物浓度的装置及方法

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