CN112924527A - Method for improving detection sensitivity of exhaled propofol - Google Patents
Method for improving detection sensitivity of exhaled propofol Download PDFInfo
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- CN112924527A CN112924527A CN201911241005.2A CN201911241005A CN112924527A CN 112924527 A CN112924527 A CN 112924527A CN 201911241005 A CN201911241005 A CN 201911241005A CN 112924527 A CN112924527 A CN 112924527A
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- OLBCVFGFOZPWHH-UHFFFAOYSA-N propofol Chemical compound CC(C)C1=CC=CC(C(C)C)=C1O OLBCVFGFOZPWHH-UHFFFAOYSA-N 0.000 title claims abstract description 40
- 229960004134 propofol Drugs 0.000 title claims abstract description 40
- 238000000034 method Methods 0.000 title claims abstract description 32
- 238000001514 detection method Methods 0.000 title claims abstract description 28
- 230000035945 sensitivity Effects 0.000 title claims abstract description 12
- 238000005070 sampling Methods 0.000 claims abstract description 68
- 239000012528 membrane Substances 0.000 claims abstract description 50
- 238000002347 injection Methods 0.000 claims abstract description 36
- 239000007924 injection Substances 0.000 claims abstract description 36
- 238000003795 desorption Methods 0.000 claims abstract description 15
- 239000004205 dimethyl polysiloxane Substances 0.000 claims abstract description 15
- 229920000435 poly(dimethylsiloxane) Polymers 0.000 claims abstract description 15
- 239000004065 semiconductor Substances 0.000 claims abstract description 15
- 238000005057 refrigeration Methods 0.000 claims abstract description 14
- -1 polydimethylsiloxane Polymers 0.000 claims abstract description 4
- 239000007789 gas Substances 0.000 claims description 18
- 239000012159 carrier gas Substances 0.000 claims description 16
- 238000001871 ion mobility spectroscopy Methods 0.000 claims description 13
- 238000010438 heat treatment Methods 0.000 claims description 6
- 230000005012 migration Effects 0.000 claims description 5
- 238000013508 migration Methods 0.000 claims description 5
- 238000001228 spectrum Methods 0.000 claims description 5
- 238000001816 cooling Methods 0.000 claims description 3
- 230000000694 effects Effects 0.000 claims description 3
- 238000005485 electric heating Methods 0.000 claims description 3
- 230000035699 permeability Effects 0.000 abstract 1
- 239000000523 sample Substances 0.000 description 48
- 239000003153 chemical reaction reagent Substances 0.000 description 7
- RDOXTESZEPMUJZ-UHFFFAOYSA-N anisole Chemical compound COC1=CC=CC=C1 RDOXTESZEPMUJZ-UHFFFAOYSA-N 0.000 description 4
- 230000003444 anaesthetic effect Effects 0.000 description 3
- 238000004458 analytical method Methods 0.000 description 3
- 238000012544 monitoring process Methods 0.000 description 3
- 238000002076 thermal analysis method Methods 0.000 description 3
- 238000010201 enrichment analysis Methods 0.000 description 2
- UZKWTJUDCOPSNM-UHFFFAOYSA-N methoxybenzene Substances CCCCOC=C UZKWTJUDCOPSNM-UHFFFAOYSA-N 0.000 description 2
- 206010002091 Anaesthesia Diseases 0.000 description 1
- 229910018503 SF6 Inorganic materials 0.000 description 1
- 230000037005 anaesthesia Effects 0.000 description 1
- 239000008280 blood Substances 0.000 description 1
- 210000004369 blood Anatomy 0.000 description 1
- 239000013068 control sample Substances 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 239000011159 matrix material Substances 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- SFZCNBIFKDRMGX-UHFFFAOYSA-N sulfur hexafluoride Chemical compound FS(F)(F)(F)(F)F SFZCNBIFKDRMGX-UHFFFAOYSA-N 0.000 description 1
- 229960000909 sulfur hexafluoride Drugs 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N27/00—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means
- G01N27/62—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means by investigating the ionisation of gases, e.g. aerosols; by investigating electric discharges, e.g. emission of cathode
- G01N27/626—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means by investigating the ionisation of gases, e.g. aerosols; by investigating electric discharges, e.g. emission of cathode using heat to ionise a gas
- G01N27/628—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means by investigating the ionisation of gases, e.g. aerosols; by investigating electric discharges, e.g. emission of cathode using heat to ionise a gas and a beam of energy, e.g. laser enhanced ionisation
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- Chemical & Material Sciences (AREA)
- Physics & Mathematics (AREA)
- Life Sciences & Earth Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Electrochemistry (AREA)
- Health & Medical Sciences (AREA)
- Optics & Photonics (AREA)
- Analytical Chemistry (AREA)
- Biochemistry (AREA)
- General Health & Medical Sciences (AREA)
- General Physics & Mathematics (AREA)
- Immunology (AREA)
- Pathology (AREA)
- Other Investigation Or Analysis Of Materials By Electrical Means (AREA)
- Sampling And Sample Adjustment (AREA)
Abstract
本发明公开了一种提高呼出气丙泊酚检测灵敏度的方法，采用低温富集高温热解析膜进样的方法，利用PDMS(聚二甲基硅氧烷)膜的疏水性和选择透过性，有效的消除了呼出气中湿度的影响，通过半导体制冷低温富集采样，高温热解析的膜进样方法，将呼出气丙泊酚检测的灵敏度提高到ppbv量级。
The invention discloses a method for improving the detection sensitivity of exhaled propofol, which adopts a low-temperature enrichment and high-temperature thermal desorption membrane injection method, and utilizes the hydrophobicity and selective permeability of PDMS (polydimethylsiloxane) membrane. , effectively eliminates the influence of humidity in exhaled breath, and improves the sensitivity of exhaled propofol detection to ppbv level by means of semiconductor refrigeration low temperature enrichment sampling and high temperature thermal desorption membrane sampling method.
Description
Technical Field
The method is based on the photoionization ion mobility spectrometry, combines with an enrichment analysis membrane sample feeding device, further eliminates the interference of humidity in the exhaled breath, improves the sensitivity of exhaled breath propofol detection, and can be used for detecting other components in the exhaled breath and high-humidity samples in the environment.
Background
The ion mobility spectrometry has high detection speed and high sensitivity, can be used for on-site rapid detection and analysis, but is easily interfered by other substances when complex matrix components are analyzed, such as humidity in exhaled breath, high-humidity environmental gas and the like. The concentration of the anesthetic propofol in the exhaled breath has certain correlation with the concentration of the anesthetic propofol in blood, and the online monitoring of the propofol in the exhaled breath anesthetic has important clinical significance for the depth monitoring of the anesthesia in the operation.
Penliking et al developed a method for simultaneously detecting NO and propofol in exhaled breath, and the collected exhaled breath and carrier gas were mixed in a mixed mode and then transferred to a sample injection port through a tetrafluoro tube without effective separation and removal of water molecules in exhaled breath, and detection of ion mobility spectrometry was complicated.
Zhouqinghua et al developed an ion mobility spectrometer that simultaneously monitored propofol and sulfur hexafluoride in exhaled breath, and continuously pumped the exhaled breath of a patient into the ion mobility spectrometer for real-time monitoring by sampling with an air pump. The expired air sample is not effectively enriched and processed, so that the signal intensity of propofol is only dozens of mV.
Therefore, the optical-electric ion mobility spectrometry of the enrichment analysis membrane sample injection is developed, the interference of humidity is eliminated, and the sensitivity of propofol detection in exhaled breath is improved.
Disclosure of Invention
The invention develops a method for improving the detection sensitivity of exhaled propofol by combining semiconductor refrigeration low-temperature enrichment sampling and high-temperature thermal desorption sample injection with reagent molecule-assisted photoionization ion mobility spectrometry.
The technical problem to be solved by the invention is as follows: eliminating the interference of humidity in the exhaled breath and improving the sensitivity of propofol detection in the exhaled breath.
The specific content comprises the following steps: a method for improving detection sensitivity of exhaled propofol adopts a membrane sample injection device as a hollow closed cavity, a PDMS (polydimethylsiloxane) membrane is arranged in the cavity and divides the cavity into two areas which are not communicated with each other, one area is a semiconductor refrigeration low-temperature enrichment sampling area, the other area is a high-temperature heating analysis membrane sample injection area, and a semiconductor refrigeration sheet for cooling the sampling area is arranged on the side wall surface of the cavity of the sampling area; an electric heating element for heating the sample injection region is arranged on the side wall surface of the cavity of the sample injection region;
a propofol sample gas inlet and a gas outlet connected with a sampling pump are arranged on the side wall surface of the cavity of the sampling area; a carrier gas inlet and a carrier gas outlet connected with the ion mobility spectrometry sample inlet are arranged on the side wall surface of the cavity of the sample injection region;
the detection specific process comprises two processes of semiconductor refrigeration low-temperature enrichment sampling and high-temperature heating analysis membrane sample introduction;
in the sampling process, the sampling area is maintained at a lower temperature, the sample gas continuously flows through the membrane sample injection device under the action of the sampling pump, and at the moment, propofol molecules are adsorbed and dissolved on the PDMS membrane, so that the enrichment effect is achieved; simultaneously, carrier gas directly enters the ion mobility spectrometry from a sample inlet;
in the membrane sample injection process, a sampling flow path of a sampling pump is cut off, the sampling pump stops working, and meanwhile, the temperature of a sample injection area of a membrane sample injection device is rapidly increased, so that propofol molecules in a PDMS membrane can be rapidly analyzed; and after the thermal desorption process is finished, switching the carrier gas to enter a sample injection area of the membrane sample injection device, and sending the desorbed propofol molecules into the IMS from a sample inlet for detection.
And after one detection period is finished, starting a semiconductor refrigerating device near the membrane sample introduction device to cool the sampling area so as to start the next detection.
The expired air enters the sampling area through a port on one side of the membrane sample introduction, and then is connected with one port of the two-position one-way electromagnetic valve through the other port on the same side, and the other port of the two-position one-way electromagnetic valve is connected with an air suction port of the sampling pump; the carrier gas flows in through one port of the three-position two-way electromagnetic valve, two ports on the other side of the three-position two-way electromagnetic valve are respectively connected with the sample inlet of the ion mobility spectrometry and one port of the sample inlet area of the membrane sample inlet device, and the other port of the membrane sample inlet area is connected with the sample inlet of the ion mobility spectrometry.
The refrigeration time of the sampling area is 100-200s, and the temperature of the sampling area is controlled to be 30-50 ℃.
The thermal analysis time is 30-60s, the temperature of the thermal analysis control sample injection region is 120 ℃, and the time of the sample injection process after the thermal analysis is 30-60 s.
The gas outlet of the ion mobility spectrometry is positioned at one end close to the reaction zone between the reaction zone and the migration zone, the flow meter of the gas outlet of the sampling pump is arranged at 600ml/min for 200-.
Drawings
Referring to fig. 1 and 2, the method relates to an ion mobility spectrometer with enriched desorption membrane sampling, wherein 1 is a membrane sampling device, 2 is an electric heating element for raising the temperature of a sampling area, 3 is a semiconductor refrigeration sheet for lowering the temperature of the sampling area, 4 is an exhalation gas, 5 is a sample carrier gas, 6 is a three-way two-position electromagnetic valve, 7 is a two-way one-position electromagnetic valve, 8 is a sampling pump, 9 is a mass flow meter, 10 is a reagent molecule carrier gas, 11 is an anisole reagent molecule, 12 is a drift gas flow inlet, and 13 is a gas outlet; wherein, fig. 1 is a semiconductor refrigeration low-temperature enrichment sampling mode, which enriches and samples propofol in exhaled breath into a sampling region in a membrane device; FIG. 2 is a thermal desorption sample injection mode, wherein a sample in a membrane sample injection cavity is purged into an ion mobility spectrometry for detection;
FIG. 3 is an ion mobility spectrum of 100% RH propofol;
FIG. 4 is a 100% RH propofol continuous trace spectrum;
FIG. 5 is a quantitative standard curve for 100% RH propofol.
Detailed Description
The invention discloses a method for improving the detection sensitivity of exhaled propofol, which is a reagent molecule-assisted photoionization ion mobility spectrometer adopting enrichment and analytic membrane for sample injection.
In the sampling process, the sampling area is maintained at a lower temperature, the sample gas continuously flows through the membrane sample injection device under the action of the sampling pump, and at the moment, propofol molecules are adsorbed and dissolved on the PDMS membrane, so that the enrichment effect is achieved; simultaneously, carrier gas directly enters the ion mobility spectrometry from a sample inlet; in the membrane sample injection process, a sampling flow path of a sampling pump is cut off, the sampling pump stops working, and meanwhile, the temperature of a sample injection area of a membrane sample injection device is rapidly increased, so that propofol molecules in a PDMS membrane can be rapidly analyzed; and after the thermal desorption process is finished, switching the carrier gas to enter a sample injection area of the membrane sample injection device, and sending the desorbed propofol molecules into the IMS from a sample inlet for detection. And after one detection period is finished, starting a semiconductor refrigerating device near the membrane sample introduction device to cool the sampling area so as to start the next detection.
Example 1
Detecting propofol in exhaled breath by utilizing a semiconductor refrigeration low-temperature enrichment and high-temperature thermal desorption membrane sample injection device combined with a reagent molecule auxiliary photoionization technology, wherein fig. 1 shows that the exhaled breath is sampled by semiconductor refrigeration low-temperature enrichment, the propofol in the exhaled breath is enriched on a PDMS (polydimethylsiloxane) membrane, thermal desorption sample injection is carried out after the enrichment is finished, the propofol enriched on the membrane is thermally analyzed and isolated, and the propofol is swept by carrier gas to enter an ion mobility spectrum for detection, as shown in fig. 3, an ion mobility spectrogram for detecting the exhaled breath propofol by enriching the desorption membrane sample injection, the migration time of anisole reagent molecules is 4.80ms, and the reduction mobility is 2.00cm2V-1s-1The migration time of the propofol obtained by detection is 6.36ms, and the reduced mobility is 1.50cm2V-1s-1. In the whole process, the product ion peak and the reagent ion peak of propofol are tracked to obtain a dynamic tracking curve as shown in fig. 4, propofol with different concentrations is detected to obtain a quantitative standard curve of 100% RH standard gas, the quantitative equation is that y is 49.13+10.12x, and the correlation coefficient is R2＝0.99。
Claims (6)
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
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| CN201911241005.2A CN112924527A (en) | 2019-12-06 | 2019-12-06 | Method for improving detection sensitivity of exhaled propofol |
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| Application Number | Priority Date | Filing Date | Title |
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| CN201911241005.2A CN112924527A (en) | 2019-12-06 | 2019-12-06 | Method for improving detection sensitivity of exhaled propofol |
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| CN112924527A true CN112924527A (en) | 2021-06-08 |
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Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103018313A (en) * | 2011-09-20 | 2013-04-03 | 中国科学院电子学研究所 | Ionic mobility spectrometer semipermeable membrane pre-enrichment sample injection method and apparatus thereof |
| WO2016107486A1 (en) * | 2014-12-31 | 2016-07-07 | 同方威视技术股份有限公司 | Detection device and detection method |
| CN108088712A (en) * | 2016-11-21 | 2018-05-29 | 中国科学院大连化学物理研究所 | A kind of expiratory air sampling apparatus and the method for sampling for the detection of direct mass spectrography |
| CN109781827A (en) * | 2017-11-13 | 2019-05-21 | 中国科学院大连化学物理研究所 | A kind of positive ion mobility spectrometry detection method of propofol in exhaled breath |
| CN209356444U (en) * | 2018-11-25 | 2019-09-06 | 中国科学院大连化学物理研究所 | A real-time on-line monitoring ion mobility spectrometer |
-
2019
- 2019-12-06 CN CN201911241005.2A patent/CN112924527A/en active Pending
Patent Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103018313A (en) * | 2011-09-20 | 2013-04-03 | 中国科学院电子学研究所 | Ionic mobility spectrometer semipermeable membrane pre-enrichment sample injection method and apparatus thereof |
| WO2016107486A1 (en) * | 2014-12-31 | 2016-07-07 | 同方威视技术股份有限公司 | Detection device and detection method |
| US20170016856A1 (en) * | 2014-12-31 | 2017-01-19 | Nuctech Company Limited | Detection apparatus and detection method |
| US10281432B2 (en) * | 2014-12-31 | 2019-05-07 | Nuctech Company Limited | Detection apparatus and detection method |
| CN108088712A (en) * | 2016-11-21 | 2018-05-29 | 中国科学院大连化学物理研究所 | A kind of expiratory air sampling apparatus and the method for sampling for the detection of direct mass spectrography |
| CN109781827A (en) * | 2017-11-13 | 2019-05-21 | 中国科学院大连化学物理研究所 | A kind of positive ion mobility spectrometry detection method of propofol in exhaled breath |
| CN209356444U (en) * | 2018-11-25 | 2019-09-06 | 中国科学院大连化学物理研究所 | A real-time on-line monitoring ion mobility spectrometer |
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