CN106324118A - Detection method for phenolic substances in saliva of smoker - Google Patents
Detection method for phenolic substances in saliva of smoker Download PDFInfo
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- CN106324118A CN106324118A CN201610641768.6A CN201610641768A CN106324118A CN 106324118 A CN106324118 A CN 106324118A CN 201610641768 A CN201610641768 A CN 201610641768A CN 106324118 A CN106324118 A CN 106324118A
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Abstract
The invention provides a detection method for phenolic substances in saliva of a smoker. A headspace-gas chromatography-mass spectrometry method is adopted to determine phenolic substances in saliva of the smoker. According to the method, 1-5 mL of saliva of the smoker is collected through a saliva collecting tube, 1-2 mL of saliva is taken and put into a headspace bottle, the headspace bottle is rapidly sealed, analysis is carried out with a headspace-gas chromatograph-mass spectrometer, and quantification is carried out with an external standard method. The detection method is suitable for simultaneous detection of phenol, p-cresol, o-cresol, m-cresol and other phenolic substances in saliva of the smoker and has the advantages of being fast, accurate, easy to implement and the like.
Description
Technical field
The invention belongs to technical field of analytical chemistry, be specifically related to a kind of be exclusively used in the inspection of aldehydes matter in smoker's saliva
Survey method.
Background technology
Phenol (phenol) is that aromatic hydrocarbon ring hydrogen is by the substituted quasi-aromatic compound of hydroxyl (OH).Simplest
Phenol is phenol.The hydrogen atom that phenolic compound refers in aromatic hydrocarbon on phenyl ring is optionally substituted by a hydroxyl group generated compound, according to it
Hydroxy number contained by molecule can be divided into monohydric phenol and polyhydric phenols.Phenolic compound all has special aromatic odor, all in weak
Acidity, the most oxidized.The toxicity of phenolic compound is with phenol as maximum, again with phenol and first in usual phenol wastewater
The content of phenol is the highest.
The character of health risk when being conducive to the explanation mankind to be exposed to this type of material for phenolic material Quality Research in saliva
And degree.Due to saliva sample not easily collecting and preservation, in saliva, aldehydes matter content is relatively low, and detection is to disturb relatively greatly, to sample
The requirement of product pre-treatment is higher, and in saliva, the detection method of aldehydes matter has no report at present, and therefore, exploitation one is exclusively used in
In smoker's saliva, the detection method of aldehydes matter is particularly important.
Summary of the invention
It is an object of the invention to provide a kind of method of aldehydes matter detection in smoker's saliva, there is quick, accurate, behaviour
Make the advantages such as simple.
The technical solution adopted in the present invention is: collects smoker's saliva 1 ~ 5 mL with saliva collection pipe, takes 1 ~ 2 mL saliva
Liquid is to ml headspace bottle, after sealing rapidly, through HS GC-GC-MS analysis, according to component peaks area quantitative.
Described headspace sampling condition is: Sample equilibration temperature is 80 ~ 90 C, and ring temperature is 90 ~ 100 C, transmission
Line temperature is 100 ~ 110 C, and PUR 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.
Described GC conditions is: chromatographic column is the special capillary column of VOC, length 60 m × internal diameter 0.32 mm ×
Thickness 1.8 m；Carrier gas is helium (He)；Injector temperature is 160 ~ 170 C；Constant current mode, post flow 1.0 ~ 1.5 mL/
Min, split ratio 10:1 ~ 15:1；Temperature programming is 40 ~ 60 C, keeps 5 ~ 10min, with the ramp of 2 ~ 5 C/min extremely
130 ~ 150 C, keep 10 ~ 20 min.
Described Mass Spectrometry Conditions is: ionization mode is electron bombardment ionization source (EI), and ion source temperature is 200 ~ 220 C, ionization
Energy is 60 ~ 80 eV, and quadrupole rod temperature is 130 ~ 160 C, Salbutamol Selected Ion Monitoring pattern, ion Selection parameter: phenol is quantitative
Ion 94, qualitative ion 66；Orthoresol quota ion 108, qualitative ion 107；Paracresol quota ion 107, qualitative ion
108；Metacresol quota ion 108, qualitative ion 79.
In the saliva of the present invention, aldehydes matter detection method has the positive effect that:
(1) step is simple, and the method gets final product sample introduction analysis after only needing collection, sampling, processes step simple, it is easy to promote；
(2) accuracy is high, greatly reduces analysans loss in purifying transfer process, adds the accurate of analysis process
Property, the relative standard deviation of phenol between 1.25% ~ 2.81%, the relative standard deviation of orthoresol between 2.59% ~ 4.98%,
The relative standard deviation of paracresol is between 1.89% ~ 4.09%, and the relative standard deviation of metacresol is between 2.64% ~ 3.61%；
(3) environmental friendliness, while improving precision of analysis, decreases the pollution to environment.
The present invention is the detection of aldehydes matter in saliva, has quick, accurate, simple operation and other advantages.
Accompanying drawing explanation
Fig. 1 is the gas chromatogram of aldehydes matter 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 orthoresol,
The chromatographic peak of 34.02min represents paracresol, and the chromatographic peak of 35.21min represents metacresol.
Detailed description of the invention
Below in conjunction with 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 should not be regarded as limiting this
Bright scope.Unreceipted concrete technology or condition person in embodiment, according to the technology described by the document in this area or condition
Or carry out according to product description.Agents useful for same or instrument unreceipted production firm person, be and can be obtained by purchase
Conventional products.
Embodiment 1
Collect smoker's saliva 1 mL with saliva collection pipe, take 1 mL saliva to ml headspace bottle, after sealing rapidly, through head space-gas phase
Chromatograph-mas spectrometer is analyzed, according to component peaks area quantitative.
Described headspace sampling condition is: Sample equilibration temperature is 80 C, and ring temperature is 90 C, and transmission line temperature is
100 C, PUR Sample equilibration time is 20min, and pressing time is 0.1 min, and inflationtime is 0.1min, sample injection time
For 0.1min.
Described GC conditions is: chromatographic column is the special capillary column of VOC, length 60 m × internal diameter 0.32 mm ×
Thickness 1.8 m；Carrier gas is helium (He)；Injector temperature is 160 C；Constant current mode, post flow 1.0mL/min, split ratio
10:1；Temperature programming is 40 C, keeps 5min, with the ramp of 2 C/min to 130 C, keeps 10min.
Described Mass Spectrometry Conditions is: ionization mode is electron bombardment ionization source (EI), and ion source temperature is 200 C, ionizing energy
For 60eV, quadrupole rod temperature is 130 C, Salbutamol Selected Ion Monitoring pattern, ion Selection parameter: phenol quota ion 94, qualitative from
Son 66；Orthoresol quota ion 108, qualitative ion 107；Paracresol quota ion 107, qualitative ion 108；Metacresol quantitatively from
Son 108, qualitative ion 79.
According to the method described above, the meansigma methods of 5 parallel determinations of phenol is 9.25 ng/mL, and relative standard deviation is
2.81%；The meansigma methods of 5 parallel determinations of orthoresol is 5.98 ng/mL, and relative standard deviation is 3.28%；Paracresol 5 times
The meansigma methods of parallel determinations is 6.84 ng/mL, and relative standard deviation is 4.09%；5 parallel determinations of metacresol
Meansigma methods is 5.48 ng/mL, and relative standard deviation is 3.29%.
Embodiment 2
Collect smoker's saliva 5 mL with saliva collection pipe, take 2 mL salivas to ml headspace bottle, after sealing rapidly, through head space-gas phase
Chromatograph-mas spectrometer is analyzed, according to component peaks area quantitative.
Described headspace sampling condition is: Sample equilibration temperature is 90 C, and ring temperature is 100 C, and transmission line temperature is
110 C, PUR Sample equilibration time is 30 min, and pressing time is 0.3 min, and inflationtime is 0.4 min, during sample introduction
Between be 0.5 min.
Described GC conditions is: chromatographic column is the special capillary column of VOC, length 60 m × internal diameter 0.32 mm ×
Thickness 1.8 m；Carrier gas is helium (He)；Injector temperature is 170 C；Constant current mode, post flow 1.5 mL/min, shunting
Compare 15:1；Temperature programming is 60 C, keeps 10min, with the ramp of 5 C/min to 150 C, keeps 20 min.
Described Mass Spectrometry Conditions is: ionization mode is electron bombardment ionization source (EI), and ion source temperature is 220 C, ionizing energy
Being 80 eV, quadrupole rod temperature is 160 C, Salbutamol Selected Ion Monitoring pattern, ion Selection parameter: phenol quota ion 94, qualitative
Ion 66；Orthoresol 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 meansigma methods of 5 parallel determinations of phenol is 8.47 ng/mL, and relative standard deviation is
1.25%；The meansigma methods of 5 parallel determinations of orthoresol is 9.58 ng/mL, and relative standard deviation is 2.59%；Paracresol 5 times
The meansigma methods of parallel determinations is 7.84 ng/mL, and relative standard deviation is 1.89%；5 parallel determinations of metacresol
Meansigma methods is 8.47 ng/mL, and relative standard deviation is 2.64%.
Embodiment 3
Collect smoker's saliva 2 mL with saliva collection pipe, take 1.5 mL salivas to ml headspace bottle, after sealing rapidly, through head space-gas
Phase chromatograph-mas spectrometer is analyzed, according to component peaks area quantitative.
Described headspace sampling condition is: Sample equilibration temperature is 70 C, and ring temperature is 95 C, and transmission line temperature is
105 C, PUR Sample equilibration time is 25 min, and pressing time is 0.2 min, and inflationtime is 0.3 min, during sample introduction
Between be 0.2 min.
Described GC conditions is: chromatographic column is the special capillary column of VOC, length 60 m × internal diameter 0.32 mm ×
Thickness 1.8 m；Carrier gas is helium (He)；Injector temperature is 165 C；Constant current mode, post flow 1.2 mL/min, shunting
Compare 12:1；Temperature programming is 50 C, keeps 8min, with the ramp of 3 C/min to 140 C, keeps 15 min.
Described Mass Spectrometry Conditions is: ionization mode is electron bombardment ionization source (EI), and ion source temperature is 210 C, ionizing energy
Being 70 eV, quadrupole rod temperature is 150 C, Salbutamol Selected Ion Monitoring pattern, ion Selection parameter: phenol quota ion 94, qualitative
Ion 66；Orthoresol 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 meansigma methods of 5 parallel determinations of phenol is 10.28ng/mL, and relative standard deviation is
2.69%；The meansigma methods of 5 parallel determinations of orthoresol is 8.47 ng/mL, and relative standard deviation is 4.98%；Paracresol 5 times
The meansigma methods of parallel determinations is 7.58 ng/mL, and relative standard deviation is 2.59%；5 parallel determinations of metacresol
Meansigma methods is 6.59 ng/mL, and relative standard deviation is 3.61%.
The ultimate principle of the present invention, principal character and advantages of the present invention have more than been shown and described.The technology of the industry
Personnel, it should be appreciated that the present invention is not restricted to the described embodiments, simply illustrating this described in above-described embodiment and description
The principle of invention, without departing from the spirit and scope of the present invention, the present invention also has various changes and modifications, and these become
Change and improvement both falls within scope of the claimed invention.Claimed scope by appending claims and
Equivalent defines.
Claims (1)
1. the method for aldehydes matter detection in smoker's saliva, it is characterised in that: collect smoker's saliva with saliva collection pipe
Liquid 1 ~ 5 mL, takes 1 ~ 2 mL saliva to ml headspace bottle, after sealing rapidly, through HS GC-GC-MS analysis, according to
Component peaks area quantitative；
Described headspace sampling condition is: Sample equilibration temperature is 80 ~ 90 C, and ring temperature is 90 ~ 100 C, transmission line temperature
Degree is 100 ~ 110 C, and PUR Sample equilibration time is 20 ~ 30 min, and pressing time is 0.1 ~ 0.3 min, inflationtime
Being 0.1 ~ 0.4 min, sample injection time is 0.1 ~ 0.5 min；
Described GC conditions is: chromatographic column is the special capillary column of VOC, length 60 m × internal diameter 0.32 mm × thickness
1.8 µ m；Carrier gas is helium (He)；Injector temperature is 160 ~ 170 C；Constant current mode, post flow 1.0 ~ 1.5 mL/min,
Split ratio 10:1 ~ 15:1；Temperature programming is 40 ~ 60 C, keeps 5 ~ 10min, with the ramp of 2 ~ 5 C/min to 130 ~
150 C, keep 10 ~ 20 min；
Described Mass Spectrometry Conditions is: ionization mode is electron bombardment ionization source (EI), and ion source temperature is 200 ~ 220 C, ionizing energy
Being 60 ~ 80 eV, quadrupole rod temperature is 130 ~ 160 C, Salbutamol Selected Ion Monitoring pattern, ion Selection parameter: phenol quota ion
94, qualitative ion 66；Orthoresol quota ion 108, qualitative ion 107；Paracresol quota ion 107, qualitative ion 108；Between
Cresol quota ion 108, qualitative ion 79.
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Cited By (5)
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| CN110045035A (en) * | 2019-04-30 | 2019-07-23 | 上海交通大学 | Gastric cancer VOC marker in saliva and its preparing the application in stomach cancer diagnosis reagent |
| CN110554119A (en) * | 2019-10-17 | 2019-12-10 | 云南中烟工业有限责任公司 | Quantitative detection method for tree moss aroma phenolic substances |
| CN110554120A (en) * | 2019-10-17 | 2019-12-10 | 云南中烟工业有限责任公司 | Detection method of tree moss aroma phenolic substances |
| CN110568107A (en) * | 2019-10-17 | 2019-12-13 | 云南中烟工业有限责任公司 | Detection method of moss phenolic substances in moss plants or extracts |
| CN110568106A (en) * | 2019-10-17 | 2019-12-13 | 云南中烟工业有限责任公司 | Quantitative detection method for turpentine substances in turpentine plants or extracts |
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Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110045035A (en) * | 2019-04-30 | 2019-07-23 | 上海交通大学 | Gastric cancer VOC marker in saliva and its preparing the application in stomach cancer diagnosis reagent |
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| CN110554119A (en) * | 2019-10-17 | 2019-12-10 | 云南中烟工业有限责任公司 | Quantitative detection method for tree moss aroma phenolic substances |
| CN110554120A (en) * | 2019-10-17 | 2019-12-10 | 云南中烟工业有限责任公司 | Detection method of tree moss aroma phenolic substances |
| CN110568107A (en) * | 2019-10-17 | 2019-12-13 | 云南中烟工业有限责任公司 | Detection method of moss phenolic substances in moss plants or extracts |
| CN110568106A (en) * | 2019-10-17 | 2019-12-13 | 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 |
| 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 |
| 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 |
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