CN107247100A - A kind of detection of fragrance component for lifting flue gas harmony and decision method - Google Patents
A kind of detection of fragrance component for lifting flue gas harmony and decision method Download PDFInfo
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Abstract
The present invention relates to a kind of detection of fragrance component for lifting flue gas harmony and decision method, belong to technical field of analytical chemistry.The detection method being related to is the content that the methylphenol of 2 methoxyl group 4 in smoker's saliva is determined using ultra performance liquid chromatography tandem mass spectrum combination method, this method is to collect 1 ~ 2mL of smoker's saliva with saliva collection pipe, after centrifugation, 0.5 ~ 1mL supernatant liquors are taken to be analyzed through ultra performance liquid chromatography tandem mass spectrum combined instrument, quantified by external standard method.The decision method being related to analyzes the content and the relation of Analyses Methods for Sensory Evaluation Results of the methylphenol of 2 methoxyl group 4 in smoker's saliva to use correlation analysis.The detection method of the present invention can be used for the measure of the content of the methylphenol of 2 methoxyl group 4 in smoker's saliva, have the advantages that sample pre-treatments are simple, easy to operate and quantitative accurate, it is easy to popularization and application.
Description
Technical field
The invention belongs to technical field of analytical chemistry, and in particular to plant the detection of the fragrance component of lifting flue gas harmony and sentence
Determine method.
Background technology
Phenolic compound is a class important substance in cigarette smoke, and the organoleptic quality with tobacco is closely related, and some have
Specific fragrance, some then make flue gas increase unusual taste, and are difficult to be mitigated by other cause pastils.Aldehydes matter is in flue gas
In have dual character, on the one hand, rudimentary phenol is such as：Phenol, benzenediol, methylphenol etc. have special penetrating odor, especially right
Eyes, respiratory mucosa, skin etc. have strong impulse and corrosiveness.On the other hand, it is also considered as aldehydes matter fragrant to tobacco
The influence that gas has also had, such as：P-methyl phenol tool astringent taste, 2,6- xylenols tool sweet taste, 4-ethyl guaiacol tool sweet tea and
Vanilla flavored, eugenol tool fragrance and dull taste, and phenol tool sweet taste and drug smell etc..With strong phenols such as fourth
Fragrant phenol, 2- methoxyl group -4- methyl-phenols etc., as one of important formula in essence.
2- methoxyl group 4- methylphenols are colourless to weak yellow liquid, are present in aniseed essential oil, refined jasmine oil, Yilan essence
It is fragrant with pungent perfume, medicine perfume, cloves, vanilla in oil, coffee, cocoa, beer, Rum, sherry, malt liquor, whiskey
Gas, available for the fumet of whiskey, the also flavoring essence such as adjustable cloves, bacon, vanilla and flavouring essence for tobacco.Therefore,
The content of 2- methoxyl group 4- methylphenols in smoker's saliva is studied, 2- methoxyl group 4- methylphenols in smoker's saliva are found
The exploitation of relation pair cigarette product and maintenance of content and Analyses Methods for Sensory Evaluation Results have great importance.
Determine different substrates, aldehydes matter is largely reported in sample, pretreatment technology have liquid-liquid extraction, column chromatography,
Derivatization etc., pretreatment process complexity is cumbersome, and easily causes the loss of aldehydes matter or by oxidation deterioration；What aldehydes matter was commonly used
Assay method has gas chromatography-mass spectrometry, high performance liquid chromatography, gas chromatography/mass spectrometry aldehydes matter
It is oxidizable or thermally decomposed, it usually needs to perform the derivatization processing, operate very cumbersome, influence the accuracy of measurement result, often
During the high effective liquid chromatography for measuring of rule, disengaging time is long, and pretreatment process is cumbersome.Have no 2- methoxyl groups 4- in saliva at present
2- methoxyl group 4- methylphenol contents in the report of methylphenol assay method, saliva are low, accordingly, it would be desirable to develop a kind of simple
Quickly, in high sensitivity, quantitative accurate saliva 2- methoxyl group 4- methylphenols assay method.
The content of the invention
It is an object of the invention to provide a kind of detection for the fragrance component 2- methoxyl group 4- methylphenols for lifting flue gas harmony
And decision method, the detection and judgement of the fragrance component 2- methoxyl group 4- methylphenols for lifting flue gas harmony in saliva, tool
There have the advantages that to be quick, accurate.
The technical solution adopted in the present invention is as follows：
A kind of detection method for the fragrance component 2- methoxyl group 4- methylphenols for lifting flue gas harmony is carried out as follows：Received with saliva
Collector collects smoker 1 ~ 2mL of saliva, after centrifugation, takes 0.5 ~ 1mL supernatant liquors to be combined through ultra performance liquid chromatography-tandem mass spectrum
Instrument is analyzed, according to component peak area quantification, detects 2- methoxyl group 4- methylphenol contents；
Described liquid phase chromatogram condition is as follows：Chromatographic column from Waters ACQUITY UPLC HSS T3 posts (1.8 μm, 2.1 ×
100 mm) or equivalent post, mobile phase is from acetonitrile/0.5-1.0% acetic acid aqueous solution=15/85,30-39 DEG C of column temperature, flow velocity
0.1-0.6mL/min, the μ L of sample size 1 ~ 5.
Described Mass Spectrometry Conditions are as follows：Ion gun：Electron spray ionisation source（ESI）, scan mode：Cation is scanned, detection
Mode：Multiple-reaction monitoring（MRM）, electron spray voltage：4000 ~ 5000 V, ion source temperature：400 ~ 600 DEG C, auxiliary gas Gas1
Pressure：0.228 ~ 0.312 MPa, aids in gas Gas2 pressure：0.344~0.425 MPa；Salbutamol Selected Ion Monitoring pattern, ion selection
Parameter：2- methoxyl group 4- methylphenols quota ion pair is 138.1/95.2, and DP voltages are 15 ~ 20V, and CE voltages are 10 ~ 15V,
CXP voltages are 1.4 ~ 1.8V；Qualitative ion pair is 123.2/55.1, and DP voltages are 18 ~ 25V, and CE voltages are 16 ~ 23V, CXP electricity
Press as 1.5 ~ 1.9V.
A kind of decision method for the fragrance component 2- methoxyl group 4- methylphenols for lifting flue gas harmony：Use correlation analysis side
The content and the relation of Analyses Methods for Sensory Evaluation Results of 2- methoxyl group 4- methylphenols in method, analysis smoker's saliva；With successive Regression point
Relation in analysis method analysis smoker's saliva between the content of 2- methoxyl group 4- methylphenols and harmony.
Beneficial effects of the present invention are as follows：
（1）, process step it is simple, only need after sample trapping, centrifugation can sample introduction analysis, component loss to be measured is less in sample；
（2）, selectivity it is good, this method is quantitative using tandem mass spectrum, reduces interfering ion, sample analysis is selectively carried
It is high.
（3）, collect 1 ~ 2mL salivas with saliva collection pipe and be easy to preserve and carry out pre-treatment, liquid phase chromatogram condition makes 2- first
Epoxide -4- methylphenols chromatographic peak keeps optimal peak type and ensures that impurity peaks interference is minimum, and Mass Spectrometry Conditions make 2- methoxyl group 4- first
The sensitivity of base phenol detection reaches most preferably.
Brief description of the drawings
Fig. 1 is saliva 2- methoxyl group 4- methylphenols and the regression figure of harmony.
Fig. 2 is the ultra performance liquid chromatography tandem mass spectrum chromatogram that embodiment 1 determines 2- methoxyl group 4- methylphenols（Its
In, retention time represents 2- methoxyl group 4- methylphenols for 5.83min chromatographic peak）.
Embodiment
With reference to technical scheme is clearly and completely described in embodiment, it is clear that described reality
It is only the example to a part of example of the invention, rather than whole to apply example.Based on the embodiment in the present invention, this area is common
The every other embodiment that technical staff is obtained under the premise of creative work is not paid, belongs to the model that the present invention is protected
Enclose.
In the examples where no specific technique or condition is specified, according to the technology or condition described by document in the art or
Person is carried out according to product description.Agents useful for same or the unreceipted production firm person of instrument, being can be by buying the normal of acquisition
Advise product.
Embodiment 1
Smoker saliva 2mL is collected with saliva collection pipe, after centrifugation, 1mL supernatant liquors are taken through ultra performance liquid chromatography-series connection matter
Combined instrument analysis is composed, according to component peak area quantification（Quantified by external standard method）, detect 2- methoxyl group 4- methylphenol contents.
Described liquid phase chromatogram condition is as follows：Chromatographic column from Waters ACQUITY UPLC HSS T3 posts (1.8 μm,
2.1 × 100 mm) or equivalent post, mobile phase is from acetic acid aqueous solution=15/85 of acetonitrile/1.0%, 39 DEG C of column temperature, flow velocity
0.6mL/min, the μ L of sample size 5.
Described Mass Spectrometry Conditions are as follows：Ion gun：Electron spray ionisation source（ESI）, scan mode：Cation is scanned, detection
Mode：Multiple-reaction monitoring（MRM）, electron spray voltage：5000 V, ion source temperature：600 DEG C, aid in gas Gas1 pressure：0.312
MPa, aids in gas Gas2 pressure：0.425 MPa；Salbutamol Selected Ion Monitoring pattern, ion selection parameter：2- methoxyl group 4- methylphenols
Quota ion pair is 138.1/95.2, and DP voltages are 20V, and CE voltages are 15V, and CXP voltages are 1.8V；Qualitative ion pair is
123.2/55.1, DP voltages are 18V, and CE voltages are 16V, and CXP voltages are 1.5V.
According to the method described above, 5 parallel determinations of same sample, the average value of 2- methoxyl group 4- methylphenols is
0.0123mg/L, relative standard deviation is 1.45%.As shown in table 1.
2- methoxyl groups 4- methylphenol content detection results in the cigarette sample smoker's saliva of table 1
Embodiment 2
Smoker saliva 1mL is collected with saliva collection pipe, after centrifugation, 0.5mL supernatant liquors are taken through ultra performance liquid chromatography-series connection
GC-MS is analyzed, according to component peak area quantification（Quantified by external standard method）, detect 2- methoxyl group 4- methylphenol contents.
Described liquid phase chromatogram condition is as follows：Chromatographic column from Waters ACQUITY UPLC HSS T3 posts (1.8 μm,
2.1 × 100 mm) or equivalent post, mobile phase is from acetic acid aqueous solution=15/85 of acetonitrile/0.5%, 30 DEG C of column temperature, flow velocity
0.1mL/min, the μ L of sample size 1.
Described Mass Spectrometry Conditions are as follows：Ion gun：Electron spray ionisation source（ESI）, scan mode：Cation is scanned, detection
Mode：Multiple-reaction monitoring（MRM）, electron spray voltage：4000 V, ion source temperature：400 DEG C, aid in gas Gas1 pressure：0.228
MPa, aids in gas Gas2 pressure：0.344MPa；Salbutamol Selected Ion Monitoring pattern, ion selection parameter：2- methoxyl group 4- methylphenols
Quota ion pair is 138.1/95.2, and DP voltages are 15V, and CE voltages are 10V, and CXP voltages are 1.4V；Qualitative ion pair is
123.2/55.1, DP voltages are 25V, and CE voltages are 23V, and CXP voltages are 1.9V.
According to the method described above, 2- methoxyl group 4- methyl in 5 samples, each sample parallel determination 5 times, each sample is selected
The average content and relative standard deviation result of 5 measure of phenol are as shown in table 2.
2- methoxyl group 4- methylphenol content detection results in the kinds of cigarettes sample smoker's saliva of table 2
Organize 7 related personnel to carry out sensory evaluation to sample, take the average value of 7 personnel evaluations, it is as a result as shown in table 3 below.
The Analyses Methods for Sensory Evaluation Results of table 3
With correlation analysis, the content of 2- methoxyl group 4- methylphenols and Analyses Methods for Sensory Evaluation Results in analysis smoker's saliva
Conspicuousness (P is presented with harmony in relation, as a result as shown in table 4,2- methoxyl group 4- methylphenols<0.05) height (| ρ |>0.7) just
Dependency relation, illustrates with the increase of 2- methoxyl groups 4- methylphenol contents in saliva, the harmony in sense organ obtain branch present with
Elevated trend.
The coefficient correlation information of 2- methoxyl group 4- methylphenols and sensory scores in the saliva of table 4
Note:* is represented in 0.01 level（Bilateral）It is upper significantly correlated.
Analyzed with Stepwise Regression Method in smoker's saliva between the content of 2- methoxyl group 4- methylphenols and harmony
Relation, obtained regression model R2For 0.9435, model P<0.01, that is, find the change of 2- methoxyl group 4- methylphenols to harmony
Score has significant contribution, as a result as shown in table 5 and Fig. 1.
The saliva 2- methoxyl group 4- methylphenols of table 5 and the stepwise regression analysis information of harmony
Claims (2)
1. a kind of detection method for the fragrance component for lifting flue gas harmony, it is characterised in that：Smoker is collected with saliva collection pipe
1 ~ 2mL of saliva, after centrifugation, takes 0.5 ~ 1mL supernatant liquors to be analyzed through ultra performance liquid chromatography-tandem mass spectrum combined instrument, according to group
Swarming area quantitative, detects 2- methoxyl group 4- methylphenol contents；
Described liquid phase chromatogram condition is as follows：Chromatographic column select 1.8 μm of Waters ACQUITY UPLC HSS T3 posts, 2.1 ×
100 mm, mobile phase selects acetonitrile/0.5-1.0% acetic acid aqueous solution=15/85,30-39 DEG C of column temperature, flow velocity 0.1-0.6mL/
Min, the μ L of sample size 1 ~ 5；
Described Mass Spectrometry Conditions are as follows：Ion gun：Electron spray ionisation source ESI, scan mode：Cation is scanned, detection mode：It is many
Reaction monitoring MRM, electron spray voltage：4000 ~ 5000 V, ion source temperature：400 ~ 600 DEG C, aid in gas Gas1 pressure：0.228
~ 0.312 MPa, aids in gas Gas2 pressure：0.344~0.425 MPa；Salbutamol Selected Ion Monitoring pattern, ion selection parameter：2- first
Epoxide 4- methylphenols quota ion pair is 138.1/95.2, and DP voltages are 15 ~ 20V, and CE voltages are 10 ~ 15V, and CXP voltages are
1.4~1.8V；Qualitative ion pair is 123.2/55.1, and DP voltages are 18 ~ 25V, and CE voltages are 16 ~ 23V, CXP voltages are 1.5 ~
1.9V。
2. a kind of decision method for the fragrance component for lifting flue gas harmony, it is characterised in that：With the lifting cigarette described in claim 1
The fragrance component 2- methoxyl group 4- methylphenols of the detection method detection of the fragrance component 2- methoxyl group 4- methylphenols of gas harmony
Analyze the content and the relation of Analyses Methods for Sensory Evaluation Results of 2- methoxyl group 4- methylphenols in smoker's saliva；Use Stepwise Regression Method
Analyze the relation between the content of 2- methoxyl group 4- methylphenols and harmony in smoker's saliva.
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| 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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| 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 |
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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 |
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