CN106324118B - The detection method of phenolic substances in a kind of smoker's saliva - Google Patents
The detection method of phenolic substances in a kind of smoker's saliva Download PDFInfo
- Publication number
- CN106324118B CN106324118B CN201610641768.6A CN201610641768A CN106324118B CN 106324118 B CN106324118 B CN 106324118B CN 201610641768 A CN201610641768 A CN 201610641768A CN 106324118 B CN106324118 B CN 106324118B
- Authority
- CN
- China
- Prior art keywords
- ion
- saliva
- temperature
- smoker
- standard deviation
- Prior art date
- Legal status (The legal status 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 status listed.)
- Active
Links
Classifications
-
- 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
Landscapes
- 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)
- Other Investigation Or Analysis Of Materials By Electrical Means (AREA)
Abstract
The present invention provides a kind of detection method of phenolic substances in smoker's saliva.The present invention is using the phenolic substances in HS GC-Mass Spectrometry measurement smoker's saliva, this method is to collect 1 ~ 5 mL of smoker's saliva with saliva collection pipe, takes 1 ~ 2 mL saliva to ml headspace bottle, rapidly after sealing, through HS GC-mass spectrometer analysis, quantified by external standard method.This detection method detects while the phenolic substancess such as phenol, paracresol, o-cresol and metacresol suitable for smoker's saliva, has quick, accurate, simple operation and other advantages.
Description
Technical field
The invention belongs to technical field of analytical chemistry, and in particular to a kind of inspection for being exclusively used in phenolic substances in smoker's saliva
Survey method.
Background technique
Phenol (phenol) is the quasi-aromatic compound that the hydrogen in fragrant hydrocarbon ring is replaced by hydroxyl (- OH).It is simplest
Phenol is phenol.Phenolic compound refers to that the hydrogen atom in aromatic hydrocarbon on phenyl ring is optionally substituted by a hydroxyl group compound generated, according to it
Hydroxy number contained by molecule can be divided into monohydric phenol and polyphenol.Phenolic compound all has special aromatic odor, in weak
Acidity is easily oxidized in the environment.The toxicity of phenolic compound is maximum with phenol, again with phenol and first in usual phenol wastewater
The content highest of phenol.
For the property of health risk when phenolic material Quality Research is conducive to illustrate that the mankind are exposed to substance of this kind in saliva
And degree.Due to saliva sample not easily collecting and preservation, aldehydes matter content is lower in saliva, and detection is that interference is larger, to sample
Product pre-treatment it is more demanding, and the detection method of phenolic substances has not been reported at present in saliva, therefore, develops one kind and is exclusively used in
The detection method of phenolic substances is particularly important in smoker's saliva.
Summary of the invention
The object of the present invention is to provide the methods that phenolic substances in a kind of smoker's saliva detects, and have quick, accurate, behaviour
Make the advantages that simple.
The technical scheme adopted by the invention is that: 1 ~ 5 mL of smoker's saliva is collected with saliva collection pipe, takes 1 ~ 2 mL saliva
Liquid is analyzed, according to component peak area quantification to ml headspace bottle rapidly after sealing through HS GC-mass spectrometer.
The headspace sampling condition are as follows: Sample equilibration temperature is 80 ~ 90 oC, and circumstance temperature degree is 90 ~ 100 oC, transmission
Line temperature is 100 ~ 110 oC, and hot melt adhesive Sample equilibration time is 20 ~ 30 min, and pressing time is 0.1 ~ 0.3 min, inflation
Time is 0.1 ~ 0.4 min, and sample injection time is 0.1 ~ 0.5 min.
The GC conditions are as follows: chromatographic column be the dedicated capillary column of VOC, 60 m of length × internal diameter, 0.32 mm ×
1.8 μm of film thickness；Carrier gas is helium (He)；Injector temperature is 160 ~ 170 oC；Constant current mode, 1.0 ~ 1.5 mL/ of column flow
Min, split ratio 10:1 ~ 15:1；Temperature programming is 40 ~ 60 oC, keeps 5 ~ 10min, is warming up to the rate of 2 ~ 5 oC/min
130 ~ 150 oC keep 10 ~ 20 min.
The Mass Spectrometry Conditions are as follows: ionization mode is electron bombardment ionization source (EI), and ion source temperature is 200 ~ 220 oC, ionization
Energy is 60 ~ 80 eV, and quadrupole rod temperature is 130 ~ 160 oC, and Salbutamol Selected Ion Monitoring mode, ion selection parameter: phenol is quantitative
Ion 94, qualitative ion 66；O-cresol quota ion 108, qualitative ion 107；Paracresol quota ion 107, qualitative ion
108；Metacresol quota ion 108, qualitative ion 79.
Phenolic substances detection method has the positive effect that in saliva of the invention:
(1) step is simple, this method only need collect, sampling after can sample introduction is analyzed, processing step is simple, easy to spread；
(2) accuracy is high, greatly reduces loss of the analysans in purification transfer process, increases analytic process
Accuracy, the relative standard deviation of phenol is between 1.25% ~ 2.81%, and the relative standard deviation of o-cresol is 2.59% ~ 4.98%
Between, the relative standard deviation of paracresol is between 1.89% ~ 4.09%, and the relative standard deviation of metacresol is 2.64% ~ 3.61%
Between；
(3) environmental-friendly, while improving precision of analysis, reduce the pollution to environment.
Detection of the present invention for phenolic substances in saliva has quick, accurate, simple operation and other advantages.
Detailed description of the invention
Fig. 1 is the gas chromatogram of phenolic substances in smoker's saliva.
Wherein, retention time is that the chromatographic peak of 29.47min represents phenol, and the chromatographic peak of 32.99min represents o-cresol,
The chromatographic peak of 34.02min represents paracresol, and the chromatographic peak of 35.21min represents metacresol.
Specific embodiment
Below with reference to embodiment, the present invention is described in further detail.
It will be understood to those of skill in the art that the following example is merely to illustrate the present invention, and it should not be regarded as limiting this hair
Bright range.In the examples where no specific technique or condition is specified, described technology or conditions according to the literature in the art
Or it is carried out according to product description.Reagents or instruments used without specified manufacturer is that can be obtained by purchase
Conventional products.
Embodiment 1
1 mL of smoker's saliva is collected with saliva collection pipe, takes 1 mL saliva to ml headspace bottle, rapidly after sealing, through head space-
Gas chromatograph-mass spectrometer (GC-MS) analysis, according to component peak area quantification.
The headspace sampling condition are as follows: Sample equilibration temperature is 80 oC, and circumstance temperature degree is 90 oC, and transmission line temperature is
100 oC, hot melt adhesive Sample equilibration time are 20min, and pressing time is 0.1 min, inflationtime 0.1min, sample injection time
For 0.1min.
The GC conditions are as follows: chromatographic column be the dedicated capillary column of VOC, 60 m of length × internal diameter, 0.32 mm ×
1.8 μm of film thickness；Carrier gas is helium (He)；Injector temperature is 160oC；Constant current mode, column flow 1.0mL/min, split ratio
10:1；Temperature programming is 40 oC, keeps 5min, is warming up to 130oC with the rate of 2 oC/min, keeps 10min.
The Mass Spectrometry Conditions are as follows: ionization mode is electron bombardment ionization source (EI), ion source temperature 200oC, ionizing energy
For 60eV, quadrupole rod temperature is 130oC, Salbutamol Selected Ion Monitoring mode, ion selection parameter: phenol quota ion 94, it is qualitative from
Son 66；O-cresol quota ion 108, qualitative ion 107；Paracresol quota ion 107, qualitative ion 108；Metacresol it is quantitative from
Sub 108, qualitative ion 79.
According to the method described above, the average value of 5 parallel determinations of phenol is 9.25 ng/mL, and relative standard deviation is
2.81%；The average value of 5 parallel determinations of o-cresol is 5.98 ng/mL, relative standard deviation 3.28%；Paracresol 5 times
The average value of parallel determinations is 6.84 ng/mL, relative standard deviation 4.09%；5 parallel determinations of metacresol
Average value is 5.48 ng/mL, relative standard deviation 3.29%.
Embodiment 2
5 mL of smoker's saliva is collected with saliva collection pipe, takes 2 mL salivas to ml headspace bottle, rapidly after sealing, through head space-
Gas chromatograph-mass spectrometer (GC-MS) analysis, according to component peak area quantification.
The headspace sampling condition are as follows: Sample equilibration temperature is 90 oC, and circumstance temperature degree is 100 oC, and transmission line temperature is
110 oC, hot melt adhesive Sample equilibration time are 30 min, and pressing time is 0.3 min, and inflationtime is 0.4 min, when sample introduction
Between be 0.5 min.
The GC conditions are as follows: chromatographic column be the dedicated capillary column of VOC, 60 m of length × internal diameter, 0.32 mm ×
1.8 μm of film thickness；Carrier gas is helium (He)；Injector temperature is 170 oC；Constant current mode, 1.5 mL/min of column flow are shunted
Compare 15:1；Temperature programming is 60 oC, keeps 10min, is warming up to 150 oC with the rate of 5 oC/min, keeps 20 min.
The Mass Spectrometry Conditions are as follows: ionization mode is electron bombardment ionization source (EI), and ion source temperature is 220 oC, ionizing energy
For 80 eV, quadrupole rod temperature is 160 oC, Salbutamol Selected Ion Monitoring mode, ion selection parameter: phenol quota ion 94, qualitative
Ion 66；O-cresol quota ion 108, qualitative ion 107；Paracresol quota ion 107, qualitative ion 108；Metacresol is quantitative
Ion 108, qualitative ion 79.
According to the method described above, the average value of 5 parallel determinations of phenol is 8.47 ng/mL, and relative standard deviation is
1.25%；The average value of 5 parallel determinations of o-cresol is 9.58 ng/mL, relative standard deviation 2.59%；Paracresol 5 times
The average value of parallel determinations is 7.84 ng/mL, relative standard deviation 1.89%；5 parallel determinations of metacresol
Average value is 8.47 ng/mL, relative standard deviation 2.64%.
Embodiment 3
2 mL of smoker's saliva is collected with saliva collection pipe, takes 1.5 mL salivas to ml headspace bottle, rapidly after sealing, through pushing up
Sky-gas chromatograph-mass spectrometer (GC-MS) analysis, according to component peak area quantification.
The headspace sampling condition are as follows: Sample equilibration temperature is 70 oC, and circumstance temperature degree is 95 oC, and transmission line temperature is
105 oC, hot melt adhesive Sample equilibration time are 25 min, and pressing time is 0.2 min, and inflationtime is 0.3 min, when sample introduction
Between be 0.2 min.
The GC conditions are as follows: chromatographic column be the dedicated capillary column of VOC, 60 m of length × internal diameter, 0.32 mm ×
1.8 μm of film thickness；Carrier gas is helium (He)；Injector temperature is 165 oC；Constant current mode, 1.2 mL/min of column flow are shunted
Compare 12:1；Temperature programming is 50 oC, keeps 8min, is warming up to 140 oC with the rate of 3 oC/min, keeps 15 min.
The Mass Spectrometry Conditions are as follows: ionization mode is electron bombardment ionization source (EI), and ion source temperature is 210 oC, ionizing energy
For 70 eV, quadrupole rod temperature is 150 oC, Salbutamol Selected Ion Monitoring mode, ion selection parameter: phenol quota ion 94, qualitative
Ion 66；O-cresol quota ion 108, qualitative ion 107；Paracresol quota ion 107, qualitative ion 108；Metacresol is quantitative
Ion 108, qualitative ion 79.
According to the method described above, the average value of 5 parallel determinations of phenol is 10.28ng/mL, and relative standard deviation is
2.69%；The average value of 5 parallel determinations of o-cresol is 8.47 ng/mL, relative standard deviation 4.98%；Paracresol 5 times
The average value of parallel determinations is 7.58 ng/mL, relative standard deviation 2.59%；5 parallel determinations of metacresol
Average value is 6.59 ng/mL, relative standard deviation 3.61%.
The basic principles, main features and advantages of the present invention have been shown and described above.The technology of the industry
Personnel are it should be appreciated that the present invention is not limited to the above embodiments, and the above embodiments and description only describe this
The principle of invention, without departing from the spirit and scope of the present invention, various changes and improvements may be made to the invention, these changes
Change and improvement all fall within the protetion scope of the claimed invention.The claimed scope of the invention by appended claims and its
Equivalent thereof.
Claims (1)
1. a kind of method that phenolic substances detects in smoker's saliva, it is characterised in that: collect smoker's saliva with saliva collection pipe
1~5mL of liquid takes 1~2mL saliva to analyze rapidly after sealing through HS GC-mass spectrometer to ml headspace bottle, according to
Component peak area quantification；
The headspace sampling condition are as follows: Sample equilibration temperature is 80~90 DEG C, and circumstance temperature degree is 90~100 DEG C, transmission line temperature
Be 100~110 DEG C, Sample equilibration time be 20~30min, pressing time be 0.1~0.3min, inflationtime be 0.1~
0.4min, sample injection time are 0.1~0.5min；
The GC conditions are as follows: chromatographic column is the dedicated capillary column of VOC, length 60m × internal diameter 0.32mm × film thickness 1.8
μm；Carrier gas is helium；Injector temperature is 160~170 DEG C；Constant current mode, 1.0~1.5mL/min of column flow, split ratio 10:1
~15:1；Temperature programming is 40~60 DEG C, keeps 5~10min, is warming up to 130~150 DEG C with the rate of 2~5 DEG C/min, protects
Hold 10~20min；
The Mass Spectrometry Conditions are as follows: ionization source is electron bombardment ionization source, and ion source temperature is 200~220 DEG C, ionizing energy is 60~
80eV, quadrupole rod temperature are 130~160 DEG C, Salbutamol Selected Ion Monitoring mode, ion selection parameter: phenol quota ion 94, qualitative
Ion 66；O-cresol quota ion 108, qualitative ion 107；Paracresol quota ion 107, qualitative ion 108；Metacresol is quantitative
Ion 108, qualitative ion 79；
Wherein, the relative standard deviation of phenol is between 1.25%~2.81%, and the relative standard deviation of o-cresol is 2.59%
Between~4.98%, between 1.89%~4.09%, the relative standard deviation of metacresol exists the relative standard deviation of paracresol
Between 2.64%~3.61%.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610641768.6A CN106324118B (en) | 2016-08-08 | 2016-08-08 | The detection method of phenolic substances in a kind of smoker's saliva |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610641768.6A CN106324118B (en) | 2016-08-08 | 2016-08-08 | The detection method of phenolic substances in a kind of smoker's saliva |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN106324118A CN106324118A (en) | 2017-01-11 |
| CN106324118B true CN106324118B (en) | 2019-01-08 |
Family
ID=57740897
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201610641768.6A Active CN106324118B (en) | 2016-08-08 | 2016-08-08 | The detection method of phenolic substances in a kind of smoker's saliva |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN106324118B (en) |
Families Citing this family (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110045035B (en) | 2019-04-30 | 2021-05-11 | 上海交通大学 | Gastric cancer VOC marker in saliva and application thereof in preparation of gastric cancer diagnostic reagent |
| CN110568107B (en) * | 2019-10-17 | 2021-08-03 | 云南中烟工业有限责任公司 | Detection method of moss phenolic substances in moss plants or extracts |
| CN110568106B (en) * | 2019-10-17 | 2021-08-03 | 云南中烟工业有限责任公司 | Quantitative detection method for turpentine substances in turpentine plants or extracts |
| CN110554119B (en) * | 2019-10-17 | 2021-08-03 | 云南中烟工业有限责任公司 | Quantitative detection method for tree moss aroma phenolic substances |
| CN110554120B (en) * | 2019-10-17 | 2021-08-03 | 云南中烟工业有限责任公司 | Detection method of tree moss fragrant ester substance |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104111296A (en) * | 2014-07-29 | 2014-10-22 | 云南中烟工业有限责任公司 | Method for detecting phenol in hot melt glue |
| CN104865338A (en) * | 2015-06-12 | 2015-08-26 | 安徽古井贡酒股份有限公司 | Method for quantificationally detecting phenolic compounds in solid-state fermentation products |
-
2016
- 2016-08-08 CN CN201610641768.6A patent/CN106324118B/en active Active
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104111296A (en) * | 2014-07-29 | 2014-10-22 | 云南中烟工业有限责任公司 | Method for detecting phenol in hot melt glue |
| CN104865338A (en) * | 2015-06-12 | 2015-08-26 | 安徽古井贡酒股份有限公司 | Method for quantificationally detecting phenolic compounds in solid-state fermentation products |
Non-Patent Citations (3)
| Title |
|---|
| Quantitative Determination of Phenols in Mainstream Smoke with Solid-Phase Microextraction-Gas Chromatography-Selected Ion Monitoring Mass Spectrometry;T.Jeffrey Clark et al;《Journal of Chromatographic Science》;19960630;第34卷;第272-275页 |
| Serban C. Moldoveanu et al.Gas chromatography/mass spectrometry versus liquid chromatography/fluorescence detection in the analysis of phenols in mainstream cigarette smoke.《Journal of Chromatography A》.2006,第1141卷 |
| 固相微萃取-气相色谱质谱法测定烟草中的酚类化合物;张艳芳 等;《化学分析计量》;20101120;第19卷(第6期);第42-44页 |
Also Published As
| Publication number | Publication date |
|---|---|
| CN106324118A (en) | 2017-01-11 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN106324118B (en) | The detection method of phenolic substances in a kind of smoker's saliva | |
| Glasius et al. | Determination of polar terpene oxidation products in aerosols by liquid chromatography–ion trap mass spectrometry | |
| CN104122358B (en) | A kind of assay method of electronic cigarette aroma volatile | |
| Schipilliti et al. | Genuineness assessment of mandarin essential oils employing gas chromatography‐combustion‐isotope ratio MS (GC‐C‐IRMS) | |
| Nhu-Trang et al. | Authenticity control of essential oils containing citronellal and citral by chiral and stable-isotope gas-chromatographic analysis | |
| Bicchi et al. | New trends in the analysis of the volatile fraction of matrices of vegetable origin: a short overview. A review. | |
| Lestremau et al. | Investigation of artefact formation during analysis of volatile sulphur compounds using solid phase microextraction (SPME) | |
| CN103076411A (en) | Analytical method for determining aromatic constituents in tea | |
| Wang et al. | Comparative analysis of essential oil components in Pericarpium Citri Reticulatae Viride and Pericarpium Citri Reticulatae by GC–MS combined with chemometric resolution method | |
| CN104865338A (en) | Method for quantificationally detecting phenolic compounds in solid-state fermentation products | |
| Risticevic et al. | Protocol for the development of automated high-throughput SPME–GC methods for the analysis of volatile and semivolatile constituents in wine samples | |
| Ma et al. | Accurate analysis of trace earthy‐musty odorants in water by headspace solid phase microextraction gas chromatography‐mass spectrometry | |
| Schäffer et al. | Forensic profiling of sassafras oils based on comprehensive two-dimensional gas chromatography | |
| Park et al. | Simple preparative gas chromatographic method for isolation of menthol and menthone from peppermint oil, with quantitative GC‐MS and 1H NMR assay | |
| Wang et al. | Qualitative analysis of flavors and fragrances added to tea by using GC–MS | |
| Cucinotta et al. | Simultaneous evaluation of the enantiomeric and carbon isotopic ratios of Cannabis sativa L. essential oils by multidimensional gas chromatography | |
| Liu et al. | Determination of highly volatile compounds in fresh onion (Allium cepa L.) by room‐temperature enrichment headspace‐trap coupled to cryotrapping GC–MS | |
| CN111679009B (en) | GC-MS/MS method for simultaneously detecting volatile and semi-volatile acids, alcohols and phenols in tobacco flavor and fragrance | |
| CN116539768A (en) | Analysis method of volatile organic compounds in hops or hops essential oil and application thereof | |
| CN106018650A (en) | Method for identifying nitrogen-containing compound in kaoliang spirit | |
| CN105510481A (en) | Detection method for 2,6-di-tert-butyl-4-methylphenol in hot melt adhesive | |
| Cao et al. | QSRR study of GC retention indices of volatile compounds emitted from Mosla chinensis Maxim by multiple linear regression | |
| CN110568101A (en) | Method for determining volatile and semi-volatile components in cut tobacco based on HS-SPME-GC-MS/MS | |
| CN111272906B (en) | Method for determining flower fragrance components in main stream smoke of cigarette | |
| Polvara et al. | Analysis of odorous VOCs using TD-GC-MS/FID/PFPD: development and applications to real samples |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| GR01 | Patent grant | ||
| GR01 | Patent grant |