CN106770760B - A kind of while separation and the method for measuring a variety of aldehydes matters in saliva - Google Patents
A kind of while separation and the method for measuring a variety of aldehydes matters in saliva Download PDFInfo
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Abstract
The present invention relates to a kind of methods of a variety of aldehydes matters in separation and measurement saliva, belong to technical field of analytical chemistry, the present invention collects saliva sample using saliva collection pipe, supernatant is taken after having acquired after high speed centrifugation, then successively it is acidified, be added internal standard, rear vortex oscillation to mixing, then miillpore filter is crossed, filtrate is detached and is measured a variety of aldehydes matters in saliva using ultra performance liquid chromatography multi-wavelength fluorescence method, makes standard curve, inner mark method ration.The method of the present invention can be effectively used for detaching and measuring a variety of aldehydes matters in saliva, and method good separating effect, detection limit is low, and precision is good, accurately and reliably, have application value.
Description
Technical field
The invention belongs to technical field of analytical chemistry, and in particular to a kind of to detach and measure simultaneously a variety of phenolic materials in saliva
The method of matter.
Background technology
Phenol, benzenediol, methylphenol etc., they not only have compared with niff, also have to skin and respiratory mucosa
Strong impulse acts on and carcinogenesis.Other phenols have strong perfume (or spice) such as eugenol, 2- methoxyl group -4- methyl-phenols
Gas is one of the important formula in essence.These aldehydes matters are largely present in cigarette mainstream flue gas, can pass through tobacco sucking
The saliva solution absorption of person, involuntary smoker, and then human body is had an impact.In addition, being largely exposed to the human body of aldehydes matter
There may be phenols in saliva, phenols is also likely to be present in a large amount of aldehydes matter poisoner's salivas for sucking aldehydes matters and causing
Substance.Therefore research measures the phenols component that dissolving is absorbed in human saliva, not only can provide number for the assessment smoked with health
According to support, it may also be used for evaluate the Exposure of aldehydes matter, or for detecting phenol poisoning.
It is largely reported currently, measuring aldehydes matter in different substrates, sample and having, however a variety of phenolic materials in saliva sample
The measurement of matter has not been reported.The common assay method of aldehydes matter has gas chromatography-mass spectrometry, high performance liquid chromatography
Method.But use gas chromatography/mass spectrometry aldehydes matter oxidizable or thermally decomposed, it usually needs performs the derivatization place
Reason, operation is very complicated, influences the accuracy of measurement result.When using conventional high effective liquid chromatography for measuring, measure simultaneously
Object it is few, disengaging time is long, and pretreatment process is cumbersome.Therefore, simple and quick, good separating effect, high throughput, height are developed
The separation of a variety of aldehydes matters and assay method are very urgent in sensitivity, quantitative accurate saliva.
Invention content
It is an object of the invention to be directed to a variety of aldehydes matter separation and method for measuring in current saliva to have no document report
The present situation and the deficiencies in the prior art in road, a kind of method for providing while separation and measuring a variety of aldehydes matters in saliva, should
Method good separating effect, detection limit is low, and precision is good, accurately and reliably, has application value, is based on realizing above-mentioned purpose,
The technical solution adopted by the present invention is as follows：
A kind of while separation and the method for measuring a variety of aldehydes matters in saliva, include the following steps：
Step (1), sample collection：Swab stick in saliva collection pipe is put in mouth, collecting pipe is put back to after chewing, through centrifugation
Afterwards, saliva sample is obtained；The chew time is 1-3min；
Step (2), sample acidification：Saliva sample is pipetted in sample cell, acidulant, internal standard compound is sequentially added, then passes through
Vortex oscillation obtains acidifying solution to being uniformly mixed；
The acidulant is acetic acid, and the acidulant dosage is the 0.5%-2% of saliva volume；
The internal standard compound is 4- fluorophenols, a concentration of 0.1-10mg/L；
Step (3) measures：The acidifying solution that step (2) is obtained crosses 0.22 μm of miillpore filter, using ultra high efficiency liquid phase color
A variety of aldehydes matters in spectrum-separation of multi-wavelength fluorescence method and measurement saliva, inner mark method ration calculate each phenol according to standard curve
The content of substance；
A variety of aldehydes matters include hydroquinone, resorcinol, adjacent methyl hydroquinone, catechol, phenol,
4- methylphenols, 2- methylphenols, 2- methoxyl group -4- methyl-phenols, 2,6- xylenols, 2- ethyl -phenols and eugenol；
The ultra high efficiency chromatographic condition is as follows：
Chromatographic column：C18 reverse-phase chromatographic columns or equivalent column, the specifications of C18 reverse-phase chromatographic columns be length × internal diameter be 100mm ×
2.1mm, grain size are 1.7 μm；Flow velocity is 0.1-0.4mL/min；Column temperature is 30-60 DEG C；Sample size is 1-3 μ L；Mobile phase A is body
The acetic acid aqueous solution of a concentration of 0.5-2% of product, Mobile phase B are the mixed solution of acetic acid, acetonitrile and water, Mobile phase B acetic acid concentration
Identical as acetic acid concentration in mobile phase A, acetonitrile volumetric concentration is 25-50%, gradient elution；
Condition of gradient elution is：0min, mobile phase A 70-95%, Mobile phase B 30-5%；6-12min is any one
Time changing mobile phase concentration proportioning, the mobile phase A after change are 0%, Mobile phase B 100%；15min stops elution；Tool
Body see the table below 1：
Table 1
| Time (min) | Mobile phase A (%) | Mobile phase B (%) |
| 0 | 70-95 | 30-5 |
| 6-12 any one moment | 0 | 100 |
| 15 | 0 | 100 |
The wavelength selection of the fluorescence detector of the multi-wavelength fluorescence method see the table below 2：
Table 2
| Compound | Excitation wavelength (nm) | Launch wavelength (nm) |
| Hydroquinone | 280-300 | 320-335 |
| Resorcinol | 270-280 | 295-315 |
| Adjacent methyl hydroquinone | 290-300 | 320-330 |
| Catechol | 270-280 | 305-320 |
| Phenol | 260-280 | 295-310 |
| 4- methylphenols | 270-280 | 300-325 |
| 2- methylphenols | 265-275 | 295-325 |
| 2- methoxyl group -4- methyl-phenols | 270-280 | 305-315 |
| 2,6- xylenols | 265-275 | 295-305 |
| 2- ethyl -phenols | 265-275 | 295-305 |
| Eugenol | 270-280 | 305-315 |
| 4- fluorophenols (internal standard) | 270-280 | 305-315 |
It is further preferred that saliva centrifugal rotational speed is not less than 10000rpm in step (1), centrifugation time is no less than
10min。
It is further preferred that the saliva amount of pipetting is 0.5-5mL in step (2).
It is further preferred that step (2) mesoscale eddies oscillation rotating speed is 500-20000rpm, the vortex oscillation time is
0.5-10min。
It is further preferred that step (3) standard curve method for drafting is as follows：Prepare a variety of aldehydes matters 5 grades are mixed
Standardization solution, concentration are respectively 0.05mg/L, 0.5mg/L, 2.5mg/L, 10mg/L, 25mg/L, in 5 grades of mixed standard solutions
It is added internal standard compound, internal standard compound concentration is identical as internal standard concentration is added in saliva sample, internal standard compound a concentration of 0.1-10mg/L, right
5 grades of mixed standard solutions carry out ultra performance liquid chromatography-multi-wavelength fluorescence methods analysis, according to each aldehydes matter respond peak area with
The ratio that internal standard compound responds peak area is ordinate, using each aldehydes matter concentration and internal standard compound concentration proportion as abscissa, is made each
The standard curve of aldehydes matter.Condition in ultra performance liquid chromatography-multi-wavelength fluorescence method analysis and aforementioned ultra high efficiency liquid phase color
Condition in spectrum-multi-wavelength fluorescence method is identical.
Compared with prior art, the present invention advantage is：
(1) the method for the present invention can effective for simultaneously detach and measure saliva in a variety of aldehydes matters, including 11 kinds not
With the phenol and benzenediol substance of substitution；
(2) sample only needs that acidification can sample introduction is analyzed, easy to operate, avoids common Solid Phase Extraction, liquid liquid extraction
It takes, object loss, oxidation, denaturation caused by the pretreatment technologies multi-step processing procedure such as derivatization or concentration, improves and survey
Determine accuracy.
(3) multi-wavelength detection is used, selectable wave-length coverage is wide, can flexibly select wave in 10-20nm wave-length coverages
It is long, and obtain high sensitivity；
(4) 4- fluorophenols is used to carry out the correction of entire analytic process as internal standard, the rate of recovery is high, quantitative accurate and reliable,
Further effectively raise accuracy.
Generally speaking, this method not only can efficiently separate and measure simultaneously a variety of aldehydes matters, Er Qiefang in saliva
Method is easy to operate, and good separating effect, detection limit is low, and precision is good, accurately and reliably, has application value.
General introduction described above for technical solution of the present invention, in order to be better understood upon the technological means of the present invention, and can
It is implemented in accordance with the contents of the specification, and in order to make above and other objects of the present invention, feature and advantage brighter
It is aobvious understandable, existing special act preferred embodiment, and coordinate attached drawing, detailed description are as follows.
Description of the drawings
Fig. 1 is the liquid chromatogram separation figure that the present invention measures more middle aldehydes matter standard solution；
Fig. 2 is the liquid chromatogram separation figure of saliva mark-on sample.
Fig. 3 is the liquid chromatogram separation figure of tobacco smokers' saliva sample.
The meaning at each peak is as follows in figure：1,1.60min, hydroquinone；2,2.41min, resorcinol；3,2.65min, it is adjacent
Methyl hydroquinone；4,3.25min, catechol；5,5.38min, phenol；6,8.36min, 4- methylphenol；7,
8.59min, 2- methylphenol；8,9.32min, 2- methoxyl group -4- methyl-phenols；9,11.37min, 2,6- xylenols；
10,11.89min, 2- ethyl -phenol；11,13.68min, eugenol；IS, 6.57min, 4- fluorophenol.
Specific implementation mode
With reference to embodiment, the present invention is described in further detail, but it is not intended to limit the present invention.
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, according to technology or condition described in document 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 buying
Conventional products.
Embodiment 1
A method of a variety of aldehydes matters in separation and measurement flue-cured tobacco smoker's saliva include the following steps：
(1) sample collection：Swab stick in saliva collection pipe is put in mouth, collecting pipe is put back to after chewing 2min, in
After centrifuging 15min under 10000rpm rotating speeds, saliva sample is obtained；
(2) sample is acidified：0.5mL saliva samples are pipetted in sample cell, 0.01mL acetic acid is added and 4- fluorophenols are added
Internal standard simultaneously makes its a concentration of 3mg/L, through vortex oscillation 2min under 2000rpm rotating speeds to be uniformly mixed；
(3) it measures：The acidifying solution that step (2) is obtained crosses miillpore filter, glimmering using ultra performance liquid chromatography-multi-wavelength
Light method measures, inner mark method ration, and object content is calculated according to standard curve.Ultra high efficiency chromatographic condition is as follows：
Chromatographic column：C18 reverse-phase chromatographic columns, specification are that length × internal diameter is 100mm × 2.1mm, and grain size is 1.7 μm；Flow velocity
For 0.3mL/min；Column temperature is 50 DEG C；Sample size is 2 μ L；Mobile phase A is the acetic acid aqueous solution that volumetric concentration is 1%, Mobile phase B
For acetic acidacetonitrile-water mixed solution, wherein acetic acid volumetric concentration 1%, acetonitrile volumetric concentration is 25%, gradient elution；
Condition of gradient elution is：0min, mobile phase A 90%, Mobile phase B 10%；10min changes flowing phase concentration
Proportioning, the mobile phase A after change are 0%, Mobile phase B 100%；15min stops elution；Condition of gradient elution see the table below 3：
Table 3
| Time (min) | Mobile phase A (%) | Mobile phase B (%) |
| 0 | 90 | 10 |
| 10 | 0 | 100 |
| 15 | 0 | 100 |
The wavelength selection of the fluorescence detector of the multi-wavelength fluorescence method see the table below 4：
Table 4
5 linearly dependent coefficient of table, precision (RSD), detection limit, quantitative limit and the rate of recovery
N indicates experiment number of repetition.
The liquid chromatogram separation figure of aldehydes matter mixed standard solution is as shown in Figure 1,11 kinds of phenols and internal standard compound have been realized
Fully separating, peak shape is sharply symmetrical；Saliva mark-on sample liquid chromatogram separation figure as shown in Fig. 2, 11 kinds of phenols and internal standard compound not
It is influenced by salivary medium, realizes and be kept completely separate；Tobacco smokers' saliva sample liquid chromatogram separation figure as shown in figure 3,
The aldehydes matter separation detected is good, is not interfered by salivary medium, can realize accurate quantitative analysis.
Table 5 gives the linearly dependent coefficient of aldehydes matter, precision in 1 method of embodiment analysis flue-cured tobacco smoker's saliva
(RSD), detection limit, quantitative limit and rate of recovery relevant parameter, above-mentioned statistics indicate that this method result is reliable, precision is good, is suitble to
The separation of aldehydes matter and measurement in flue-cured tobacco smoker's saliva.
Embodiment 2
A method of a variety of aldehydes matters in separation and measurement cigar smoker's saliva include the following steps：
(1) sample collection：Swab stick in saliva collection pipe is put in mouth, collecting pipe is put back to after chewing 1min, in
After centrifuging 12min under 12000rpm rotating speeds, saliva sample is obtained；
(2) sample is acidified：2.0mL saliva samples are pipetted in sample cell, 0.03mL acetic acid is added and 4- fluorophenols are added
Internal standard simultaneously makes its a concentration of 1.5mg/L, through vortex oscillation 0.5min under 20000rpm rotating speeds to be uniformly mixed；
(3) it measures：The acidifying solution that step (2) is obtained crosses miillpore filter, glimmering using ultra performance liquid chromatography-multi-wavelength
Light method measures, inner mark method ration, and object content is calculated according to standard curve.
Ultra high efficiency chromatographic condition is as follows：
Chromatographic column：C18 reverse-phase chromatographic columns, specification are that length × internal diameter is 100mm × 2.1mm, and grain size is 1.7 μm；Flow velocity
For 0.1mL/min；Column temperature is 30 DEG C；Sample size is 3 μ L；Mobile phase A is the acetic acid aqueous solution that volumetric concentration is 1.5%, flowing
Phase B is acetic acidacetonitrile-water mixed solution, wherein acetic acid volumetric concentration 1.5%, and acetonitrile volumetric concentration is 50%, gradient elution；
Condition of gradient elution is：0min, mobile phase A 70%, Mobile phase B 30%；6min changes flowing phase concentration
Proportioning, the mobile phase A after change are 0%, Mobile phase B 100%；15min stops elution；Condition of gradient elution see the table below 6：
Table 6
| Time (min) | Mobile phase A (%) | Mobile phase B (%) |
| 0 | 70 | 30 |
| 6 | 0 | 100 |
| 15 | 0 | 100 |
The wavelength selection of the fluorescence detector of the multi-wavelength fluorescence method see the table below 7：
Table 7
8 linearly dependent coefficient of table, precision (RSD), detection limit, quantitative limit and the rate of recovery
N indicates experiment number of repetition.
Table 8 gives the linearly dependent coefficient of aldehydes matter, precision in 2 method of embodiment analysis cigar smoker's saliva
(RSD), detection limit, quantitative limit and rate of recovery relevant parameter are spent, above-mentioned precision is good statistics indicate that this method result is reliable, fits
Separation together in aldehydes matter in cigar smoker's saliva and measurement.
Embodiment 3
A method of a variety of aldehydes matters in separation and measurement composition person's saliva include the following steps：
(1) sample collection：Swab stick in saliva collection pipe is put in mouth, collecting pipe is put back to after chewing 3min, in
After centrifuging 10min under 15000rpm rotating speeds, saliva sample is obtained；
(2) sample is acidified：5.0mL saliva samples are pipetted in sample cell, 0.025mL acetic acid is added and 4- fluorobenzene is added
Phenol internal standard simultaneously makes its a concentration of 10mg/L, through vortex oscillation 10min under 500rpm rotating speeds to be uniformly mixed；
(3) it measures：The acidifying solution that step (2) is obtained crosses miillpore filter, glimmering using ultra performance liquid chromatography-multi-wavelength
Light method measures, inner mark method ration, and object content is calculated according to standard curve.
Ultra high efficiency chromatographic condition is as follows：
Chromatographic column：C18 reverse-phase chromatographic columns, specification are that length × internal diameter is 100mm × 2.1mm, and grain size is 1.7 μm；Flow velocity
For 0.25mL/min；Column temperature is 30 DEG C；Sample size is 1 μ L；Mobile phase A is the acetic acid aqueous solution that volumetric concentration is 0.5%, flowing
Phase B is acetic acidacetonitrile-water mixed solution, wherein acetic acid volumetric concentration 0.5%, and acetonitrile volumetric concentration is 40%, gradient elution；
Condition of gradient elution is：0min, mobile phase A 95%, Mobile phase B 5%；9min changes flowing phase concentration and matches
Than the mobile phase A after change is 0%, Mobile phase B 100%；15min stops elution；Condition of gradient elution see the table below 9：
Table 9
| Time (min) | Mobile phase A (%) | Mobile phase B (%) |
| 0 | 95 | 5 |
| 9 | 0 | 100 |
| 15 | 0 | 100 |
The wavelength selection of the fluorescence detector of the multi-wavelength fluorescence method see the table below 10：
Table 10
| Time (min) | Excitation wavelength (nm) | Launch wavelength (nm) |
| Hydroquinone | 300 | 335 |
| Resorcinol | 280 | 315 |
| Adjacent methyl hydroquinone | 300 | 330 |
| Catechol | 280 | 320 |
| Phenol | 280 | 310 |
| 4- methylphenols | 280 | 325 |
| 2- methylphenols | 275 | 325 |
| 2- methoxyl group -4- methyl-phenols | 280 | 315 |
| 2,6- xylenols | 275 | 305 |
| 2- ethyl -phenols | 275 | 305 |
| Eugenol | 280 | 315 |
| 4- fluorophenols (internal standard) | 280 | 315 |
11 linearly dependent coefficient of table, precision (RSD), detection limit, quantitative limit and the rate of recovery
N indicates experiment number of repetition.
Table 11 gives the linearly dependent coefficient of aldehydes matter, precision in 3 method of embodiment analysis composition person's saliva
(RSD), detection limit, quantitative limit and rate of recovery relevant parameter are spent, above-mentioned precision is good statistics indicate that this method result is reliable, fits
Separation together in aldehydes matter in composition person's saliva and measurement.
Embodiment 4
A method of a variety of aldehydes matters in buccal cigarette eater are detached and measured, are included the following steps：
(1) sample collection：Swab stick in saliva collection pipe is put in mouth, collecting pipe is put back to after chewing 2.5min, in
After centrifuging 10min under 20000rpm rotating speeds, saliva sample is obtained；
(2) sample is acidified：3.0mL saliva samples are pipetted in sample cell, 0.03mL acetic acid is added and 4- fluorophenols are added
Internal standard simultaneously makes its a concentration of 0.1mg/L, through vortex oscillation 1min under 15000rpm rotating speeds to be uniformly mixed；
(3) it measures：The acidifying solution that step (2) is obtained crosses miillpore filter, glimmering using ultra performance liquid chromatography-multi-wavelength
Light method measures, inner mark method ration, and object content is calculated according to standard curve.
Ultra high efficiency chromatographic condition is as follows：
Chromatographic column：C18 reverse-phase chromatographic columns, specification are that length × internal diameter is 100mm × 2.1mm, and grain size is 1.7 μm；Flow velocity
For 0.2mL/min；Column temperature is 30 DEG C；Sample size is 1 μ L；Mobile phase A is the acetic acid aqueous solution that volumetric concentration is 2%, Mobile phase B
For acetic acidacetonitrile-water mixed solution, wherein acetic acid volumetric concentration 2%, acetonitrile volumetric concentration is 35%, gradient elution；
Condition of gradient elution is：0min, mobile phase A 80%, Mobile phase B 20%；12min changes flowing phase concentration
Proportioning, the mobile phase A after change are 0%, Mobile phase B 100%；15min stops elution；Condition of gradient elution see the table below
12：
Table 12
| Time (min) | Mobile phase A (%) | Mobile phase B (%) |
| 0 | 80 | 20 |
| 12 | 0 | 100 |
| 15 | 0 | 100 |
The wavelength selection of the fluorescence detector of the multi-wavelength fluorescence method see the table below 13：
Table 13
| Time (min) | Excitation wavelength (nm) | Launch wavelength (nm) |
| Hydroquinone | 290 | 330 |
| Resorcinol | 278 | 310 |
| Adjacent methyl hydroquinone | 295 | 325 |
| Catechol | 278 | 318 |
| Phenol | 275 | 308 |
| 4- methylphenols | 277 | 320 |
| 2- methylphenols | 272 | 321 |
| 2- methoxyl group -4- methyl-phenols | 278 | 312 |
| 2,6- xylenols | 272 | 302 |
| 2- ethyl -phenols | 272 | 302 |
| Eugenol | 278 | 312 |
| 4- fluorophenols (internal standard) | 278 | 312 |
14 linearly dependent coefficient of table, precision (RSD), detection limit, quantitative limit and the rate of recovery
N indicates experiment number of repetition.
Table 14 gives the linearly dependent coefficient of aldehydes matter, essence in 4 method of embodiment analysis buccal cigarette eater's saliva
Density (RSD), detection limit, quantitative limit and rate of recovery relevant parameter, above-mentioned statistics indicate that this method result is reliable, precision is good,
It is suitable for the separation of aldehydes matter and measurement in buccal cigarette eater's saliva.
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 (5)
1. a kind of while separation and the method for measuring a variety of aldehydes matters in saliva, which is characterized in that include the following steps：
Step（1）, sample collection：Swab stick in saliva collection pipe is put in mouth, collecting pipe is put back to after chewing, after centrifugation,
Obtain saliva sample；The chew time is 1-3 min；
Step（2）, sample acidification：Saliva sample is pipetted in sample cell, sequentially adds acidulant, internal standard compound, then through being vortexed
Oscillation obtains acidifying solution to being uniformly mixed；
The acidulant is acetic acid, and the acidulant dosage is the 0.5%-2% of saliva volume；
The internal standard compound is 4- fluorophenols, a concentration of 0.1-10mg/L；
Step（3）, measure：By step（2）Obtained acidifying solution crosses 0.22 μm of miillpore filter, using ultra performance liquid chromatography-
Multi-wavelength fluorescence method detaches and measures a variety of aldehydes matters in saliva, and inner mark method ration calculates each phenols according to standard curve
The content of substance；
A variety of aldehydes matters include hydroquinone, resorcinol, adjacent methyl hydroquinone, catechol, phenol, 4- first
Base phenol, 2- methylphenols, 2- methoxyl group -4- methyl-phenols, 2,6- xylenols, 2- ethyl -phenols and eugenol；
The ultra high efficiency chromatographic condition is as follows：
Chromatographic column：C18 reverse-phase chromatographic columns, it is the mm of 100 mm × 2.1, grain that the specification of C18 reverse-phase chromatographic columns, which is length × internal diameter,
Diameter is 1.7 μm；Flow velocity is 0.1-0.4 mL/min；Column temperature is 30-60 DEG C；Sample size is 1-3 μ L；Mobile phase A is that volume is dense
Degree is the acetic acid aqueous solution of 0.5-2%, and Mobile phase B is the mixed solution of acetic acid, acetonitrile and water, Mobile phase B acetic acid concentration and flowing
Acetic acid concentration is identical in phase A, and acetonitrile volumetric concentration is 25-50%, gradient elution；
Condition of gradient elution is：0min, mobile phase A 70-95%, Mobile phase B 30-5%；6-12min any one moment changes
Become flowing phase concentration proportioning, the mobile phase A after change is 0%, Mobile phase B 100%；15min stops elution；
The wavelength selection of the fluorescence detector of the multi-wavelength fluorescence method see the table below：
。
2. according to claim 1 while separation and the method for measuring a variety of aldehydes matters in saliva, it is characterised in that：Step
Suddenly（1）Middle saliva centrifugal rotational speed is not less than 10000 rpm, and centrifugation time is no less than 10 min.
3. according to claim 1 while separation and the method for measuring a variety of aldehydes matters in saliva, it is characterised in that：Step
Suddenly（2）The middle saliva amount of pipetting is 0.5-5 mL.
4. according to claim 1 while separation and the method for measuring a variety of aldehydes matters in saliva, it is characterised in that：Step
Suddenly（2）It is 500-20000 rpm that mesoscale eddies, which vibrates rotating speed, and the vortex oscillation time is 0.5-10 min.
5. the method for detaching simultaneously according to any one of claims 1-4 and measuring a variety of aldehydes matters in saliva,
It is characterized in that：Step（3）Standard curve method for drafting is as follows：Prepare 5 grades of mixed standard solutions of a variety of aldehydes matters, concentration
Internal standard is added in 5 grades of mixed standard solutions in respectively 0.05 mg/L, 0.5 mg/L, 2.5 mg/L, 10 mg/L, 25 mg/L
Object, internal standard compound concentration is identical as internal standard concentration is added in saliva sample, a concentration of 0.1-10mg/L of internal standard compound, to 5 grades of mixing marks
Quasi- solution carries out ultra performance liquid chromatography-multi-wavelength fluorescence method analysis, and respond peak area according to each aldehydes matter rings with internal standard compound
It is that ordinate makees each aldehydes matter using each aldehydes matter concentration and internal standard compound concentration proportion as abscissa to answer the ratio of peak area
Standard curve.
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| 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 |
| 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 |
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| CN101592638B (en) * | 2008-05-30 | 2012-05-09 | 贵州中烟工业公司 | Method for separating and detecting harmful phenols in main stream smoke of cigarettes |
| US8530228B2 (en) * | 2010-12-28 | 2013-09-10 | Bexmart | Integrated versatile and systems preparation of specimens |
| CN104597169B (en) * | 2015-02-16 | 2016-08-24 | 国家烟草质量监督检验中心 | For measuring the method for major phenolic compound content in electronic cigarette suction aerosol |
| CN106053648B (en) * | 2016-06-07 | 2018-07-24 | 云南中烟工业有限责任公司 | A kind of pretreating device of aldehydes matter detection and application |
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