CN111398462A - Detection method for detecting phenols and amines in exhaled air of human body - Google Patents

Detection method for detecting phenols and amines in exhaled air of human body Download PDF

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Publication number
CN111398462A
CN111398462A CN202010252956.6A CN202010252956A CN111398462A CN 111398462 A CN111398462 A CN 111398462A CN 202010252956 A CN202010252956 A CN 202010252956A CN 111398462 A CN111398462 A CN 111398462A
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China
Prior art keywords
filler
human body
exhaled
amines
stationary phase
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CN202010252956.6A
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Chinese (zh)
Inventor
孙梦
赵伟军
章旭日
温铁芳
史夏青
周伟
汪小知
张厚德
郝雷
段兴斌
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Biruisi Hangzhou Technology Co ltd
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Biruisi Hangzhou Technology Co ltd
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Priority to CN202010252956.6A priority Critical patent/CN111398462A/en
Publication of CN111398462A publication Critical patent/CN111398462A/en
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    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
    • G01N30/02—Column chromatography
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
    • G01N30/02—Column chromatography
    • G01N30/04—Preparation or injection of sample to be analysed
    • G01N30/06—Preparation
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
    • G01N30/02—Column chromatography
    • G01N30/04—Preparation or injection of sample to be analysed
    • G01N2030/042—Standards
    • G01N2030/047—Standards external
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
    • G01N30/02—Column chromatography
    • G01N30/04—Preparation or injection of sample to be analysed
    • G01N30/06—Preparation
    • G01N2030/067—Preparation by reaction, e.g. derivatising the sample

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  • Physics & Mathematics (AREA)
  • Health & Medical Sciences (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Chemical & Material Sciences (AREA)
  • Analytical Chemistry (AREA)
  • Biochemistry (AREA)
  • General Health & Medical Sciences (AREA)
  • General Physics & Mathematics (AREA)
  • Immunology (AREA)
  • Pathology (AREA)
  • Investigating Or Analysing Biological Materials (AREA)

Abstract

The invention provides a detection method for detecting phenols and amines in human exhaled breath, and belongs to the field of sample treatment. The method solves the problems that the content of phenols and amines in the exhaled air of the human body cannot be quantitatively detected at present, and the like, and the method for detecting the phenols and amines in the exhaled air of the human body comprises the following steps: collecting gas exhaled by a human body; introducing the gas exhaled by the human body into a water absorption device filled with a drying agent, and removing water in the exhaled gas; connecting an adsorption device behind the water absorption device to generate derivatization reaction; eluting the adsorption device with an eluent; detecting the eluted solution; the adsorption device is filled with a stationary phase, a derivatization reagent is attached to the stationary phase, and the chemical formula of the derivatization reagent is R-SO2-Cl. The invention has the advantages of high sensitivity, high accuracy and quantitative detection.

Description

Detection method for detecting phenols and amines in exhaled air of human body
Technical Field
The invention belongs to the field of sample treatment, and particularly relates to a detection method for detecting phenols and amines in exhaled breath of a human body.
Background
The exhaled air of human body is directly exhaled by lung, and the exhaled air of normal person is collected by pauling et al in 1971 at first, and 250 volatile organic compounds are detected.
Volatile organic compounds in exhaled air of a human body are closely related to diagnosis of diseases, the volatile organic compounds comprise phenols and amines, if phenols and amines are detected in exhaled air, the fact that the human body may have a certain disease such as lung cancer is represented, and the contents of phenols and amines in exhaled air can represent the severity of the disease to a certain extent, and subsequent further diagnosis is needed for diagnosis of the disease. But the detection of phenols and amines in the exhaled breath of the human body at the early stage is a non-invasive detection and has important significance for preventing early diseases.
For the volatile components of the exhaled breath, the components of the sample are complex, the general adsorption process is simple physical adsorption, and most of the volatile components in the exhaled breath are adsorbed on the filler by adopting an adsorbent containing a certain filler and cannot be selectively adsorbed. Therefore, most of the existing detections in the exhaled breath of human bodies are qualitative detections, which are uniformly measured after being collected, and the existing substances are judged according to different peak maps, so that the contents of phenols and amines cannot be quantitatively detected.
Disclosure of Invention
The invention aims to provide a method for detecting phenols and amines in exhaled breath of a human body, aiming at the problems in the prior art.
The first object of the present invention can be achieved by the following technical solutions: a detection method for detecting phenols and amines in exhaled breath of a human body is characterized by comprising the following steps:
s01: collecting gas exhaled by a human body;
s02: introducing the gas exhaled by the human body into a water absorption device filled with a drying agent, and removing water in the exhaled gas;
s03: connecting an adsorption device behind the water absorption device to generate derivatization reaction;
s04: eluting the adsorption device with an eluent;
s05: detecting the eluted solution;
the adsorption device is filled with a stationary phase, a derivative reagent is attached to the stationary phase, and the chemical formula of the derivative reagent is R-SO2-Cl。
Preferably, the derivatizing agent is dansyl chloride.
Preferably, the drying agent is 200mg of anhydrous sodium sulfate, and the anhydrous sodium sulfate is heated and baked at a high temperature of 500 ℃ for 4 hours to remove water, taken out and then screened by a 200-mesh screen.
Preferably, the eluent is acetonitrile, and the acetonitrile is chromatographically pure carbofuran acetonitrile or Honeywell acetonitrile.
Preferably, the reaction temperature of step S03 is between 45 and 60 ℃.
Preferably, the adsorption device is an adsorption column, and the preparation method of the adsorption column comprises the following steps:
(1) preparing a coating liquid containing a derivatization reagent and having a content of 5% by using acetonitrile as the derivatization reagent;
(2) filling a stationary phase filler on a blank adsorption column;
(3) coating the coating liquid on an adsorption column filled with a stationary phase, blow-drying by using nitrogen, and sealing and refrigerating at 4 ℃;
the preparation process is carried out in an environment with phenolic detection requirement of less than or equal to 0.25 mu g (calculated by phenol) and amine detection requirement of less than or equal to 0.1 mu g (calculated by propylamine).
Preferably, the stationary phase is selected from silica gel packing, C18One or any combination of filler and flory diatomite filler.
Preferably, silica gel filler and C18The ratio of the filler is 1:1, or the ratio of the silica gel filler to the Flori diatomite filler is 1:1, or C18The ratio of the filler to the Flori diatomite filler is 1:1, or the silica gel filler and the filler C18The ratio of filler to flory diatomaceous earth filler was 1:1: 1.
Preferably, a silica gel filler, C18The particle size of the filler and the Flori diatomite filler is 50-500 meshes.
Compared with the prior art, the invention has the following advantages:
1. the invention aims at the quantitative detection of phenols and amines in gas, and the derivatization reagent selected by the invention is coated on the stationary phase of the adsorption column by the preparation method of the adsorption column. The derivatization reagent can generate derivatization reaction with phenols and amines to generate a new derivatization product, and the chemical formula of the product is dansyl-phenol substance (C)12H12NSO2-O-C6H5-R), and dansyl-amine (C)12H12NSO2-NH-R or C12H12NSO2-N-R1R2). On one hand, the derivative product has the fluorescent characteristic, and can be detected by a sampling fluorescence detector, so that the detection sensitivity is improved. On the other hand, the molecular structure of the derivative product is enlarged, the stability is enhanced, mass spectrum detection can be adopted, and the detection sensitivity is improved.
2. The derivative reagent selected by the invention is coated on the stationary phase of the adsorption column, can selectively absorb phenolic substances and amine substances in the exhaled air of a human body, is eluted by using an eluent, and can express the contents of the phenolic substances and the amine substances in the exhaled air by detecting the content of the derivative product. The invention can quantitatively detect the contents of phenolic substances and amine substances in exhaled breath of human bodies and adopts a derivatization reagent (with the chemical formula of R-SO) containing specific groups2-Cl, wherein R represents a substituent), the process of the inventionThe selectivity should be high. The adsorption column prepared by the invention can not absorb other substances in the exhaled breath, and only aims at the phenols and amines substances, so that the final quantitative detection is more accurate.
3. The derivative reagent of the invention adopts dansyl chloride which can be adsorbed on the stationary phase, and the gaseous volatile phenols, amines and the derivative reagent coated on the stationary phase have chemical reaction and have continuity, and the produced product can be eluted from the stationary phase.
4. The stationary phase of the invention is selected from silica gel filler and C18One or any combination of filler and flory diatomite filler. And the grain diameter of the filler is 50-500 meshes. The stationary phase can well adsorb the derivatization reagent, and is favorable for eluting a product generated by the reaction of the derivatization reagent and phenols and amine substances by acetonitrile.
5. The reaction temperature of step S02 of the present invention is between 45-60 ℃. Is beneficial to the full reaction of the phenolic substances, the amine substances and the derivatization reagent in the gas.
6. The preparation process of the adsorption column is carried out in an environment with the requirement of less than or equal to 0.25 mu g (calculated by phenol) for phenol detection and less than or equal to 0.1 mu g (calculated by propylamine) for amine detection. In the environment, the phenol substances and the amine substances are basically not present in the air, and the purpose is to prevent the phenol substances and the amine substances existing in the air from reacting with the derivative reagent in the coating process, so that the experimental error is large, and the detection is not accurate.
Detailed Description
The following are specific examples of the present invention and further describe the technical solutions of the present invention, but the present invention is not limited to these examples.
The water absorption device includes but is not limited to a water absorption column, and the adsorption device includes but is not limited to an adsorption column.
Example 1
The apparatus used was: a liquid chromatography tandem mass spectrometer equipped with an Electrospray (ESI) ion source. A solid phase extraction system, a nitrogen blow-drying instrument and the like.
Firstly, coating a blank adsorption column containing a stationary phase material with a coating liquid prepared to contain dansyl chloride of 5% in an environment with the requirements of phenol detection of less than or equal to 0.25 mug (calculated by phenol) and amine detection of less than or equal to 0.1 mug (calculated by propylamine), wherein the coating liquid is coated on the blank adsorption column, and the filled stationary phase filler is 200 mg. The coating method is carried out by adopting a direct coating method. Before coating, the blank adsorption column is firstly rinsed by acetonitrile, a rinsed acetonitrile reagent is removed by a negative pressure solid phase extraction system, then 5 percent of coating liquid is directly coated on the adsorption column, after the coating is saturated, the redundant coating liquid is removed by the negative pressure solid phase extraction system to prepare a selective adsorption column capable of selectively adsorbing exhaled phenols and amines, the adsorption column is dried by nitrogen and is sealed and stored at 4 ℃ for standby application.
Collecting gas 3L-10L exhaled by a human body in a sampling bag, introducing the collected exhaled gas into an adsorption column, reacting phenols and amines in the exhaled gas with dansyl chloride coated on a stationary phase to generate a product, eluting with acetonitrile, fixing the volume of the eluted solution to 2m L, carrying out quantitative detection with L C/MS/MS, carrying out accurate quantification with an external standard working curve method, and calculating the actual content by substituting the measured peak area result into a standard working curve.
The stationary phase can be selected from silica gel filler and C18One or any combination of filler and flory diatomite filler.
The specific embodiments described herein are merely illustrative of the spirit of the invention. Various modifications or additions may be made to the described embodiments or alternatives may be employed by those skilled in the art without departing from the spirit or ambit of the invention as defined in the appended claims.

Claims (9)

1. A detection method for detecting phenols and amines in exhaled breath of a human body is characterized by comprising the following steps:
s01: collecting gas exhaled by a human body;
s02: introducing the gas exhaled by the human body into a water absorption device filled with a drying agent, and removing water in the exhaled gas;
s03: connecting an adsorption device behind the water absorption device to generate derivatization reaction;
s04: eluting the adsorption device with an eluent;
s05: detecting the eluted solution;
the adsorption device is filled with a stationary phase, a derivative reagent is attached to the stationary phase, and the chemical formula of the derivative reagent is R-SO2-Cl。
2. The method of claim 1, wherein the derivatizing reagent is dansyl chloride.
3. The method of claim 1, wherein the desiccant is 200mg of anhydrous sodium sulfate, and the anhydrous sodium sulfate is baked at a high temperature of 500 ℃ for removing water for 4 hours, and then taken out and screened with a 200-mesh screen.
4. The method of claim 1, wherein the eluent is acetonitrile, and the acetonitrile is chromatographically pure carbofuran acetonitrile or Honeywell acetonitrile.
5. The method for detecting phenolic and amine substances in exhaled breath of human body according to claim 1, wherein the reaction temperature of step S03 is 45-60 ℃.
6. The method for detecting phenols and amines in exhaled breath of human body according to claim 1, wherein said adsorption device is an adsorption column, and said adsorption column is prepared by the following steps:
(1) preparing a coating liquid containing a derivatization reagent and having a content of 5% by using acetonitrile as the derivatization reagent;
(2) filling a stationary phase filler on a blank adsorption column;
(3) coating the coating liquid on an adsorption column filled with a stationary phase, blow-drying by using nitrogen, and sealing and refrigerating at 4 ℃;
the preparation process is carried out in an environment with phenolic detection requirement of less than or equal to 0.25 mu g (calculated by phenol) and amine detection requirement of less than or equal to 0.1 mu g (calculated by propylamine).
7. The method as claimed in claim 1, wherein the stationary phase is selected from silica gel filler and C18One or any combination of filler and flory diatomite filler.
8. The method as claimed in claim 6, wherein the silica gel filler and C are added18The ratio of the filler is 1:1, or the ratio of the silica gel filler to the Flori diatomite filler is 1:1, or C18The ratio of the filler to the Flori diatomite filler is 1:1, or the silica gel filler and the filler C18The ratio of filler to flory diatomaceous earth filler was 1:1: 1.
9. The method for detecting phenols and amines in exhaled breath of human body according to claim 6, wherein silica gel filler and C18The particle size of the filler and the Flori diatomite filler is 50-500 meshes.
CN202010252956.6A 2020-04-02 2020-04-02 Detection method for detecting phenols and amines in exhaled air of human body Pending CN111398462A (en)

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Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US20070290174A1 (en) * 2004-09-30 2007-12-20 Arnold Stephen C Lactam polymer derivatives
CN103822998A (en) * 2012-11-19 2014-05-28 中国科学院大连化学物理研究所 Method for analyzing amine substances in dansyl chloride derived-plasma based on liquid chromatography mass spectrometry
CN110887910A (en) * 2019-12-12 2020-03-17 上海阿趣生物科技有限公司 Polyamine and detection method of synthetic pathway substance thereof

Patent Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US20070290174A1 (en) * 2004-09-30 2007-12-20 Arnold Stephen C Lactam polymer derivatives
CN103822998A (en) * 2012-11-19 2014-05-28 中国科学院大连化学物理研究所 Method for analyzing amine substances in dansyl chloride derived-plasma based on liquid chromatography mass spectrometry
CN110887910A (en) * 2019-12-12 2020-03-17 上海阿趣生物科技有限公司 Polyamine and detection method of synthetic pathway substance thereof

Non-Patent Citations (2)

* Cited by examiner, † Cited by third party
Title
YUMEI LIN等: "Protocol for Collection and HPLC Analysis of Volatile Carbonyl Compounds in Breath", 《CLINICAL CHEMISTRY》 *
夏同伟等: "高效液相色谱-串联质谱法测定人尿液中5种酚类内分泌干扰物", 《分析测试学报》 *

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Application publication date: 20200710