CN108037201A - The detection method of aldehyde material in a kind of processing method of buccal cigarette sample, buccal cigarette - Google Patents
The detection method of aldehyde material in a kind of processing method of buccal cigarette sample, buccal cigarette Download PDFInfo
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- CN108037201A CN108037201A CN201711288756.0A CN201711288756A CN108037201A CN 108037201 A CN108037201 A CN 108037201A CN 201711288756 A CN201711288756 A CN 201711288756A CN 108037201 A CN108037201 A CN 108037201A
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Abstract
The present invention relates to a kind of detection method of aldehyde material in processing method of buccal cigarette sample, buccal cigarette, belong to smoke-free tobacco product chromatography analysis detection technique field.The processing method of the buccal cigarette sample of the present invention, comprises the following steps：Sequentially add acidic ph modifier, derivatization reagent and extractant into buccal cigarette sample to be uniformly mixed, stratification, takes upper organic phase as sample to be tested；The volume of extractant is used as 8~15ml per 1g buccal cigarettes correspondence.The processing method of the buccal cigarette sample of the present invention, it can either accelerate to leach the aldehyde material in buccal cigarette, shorten aldehyde material and the time of derivatization reagent reaction in buccal cigarette, it can also realize that the product after reaction is carried out extraction enters organic phase at the same time, further shorten the time of analysis detection, loss of the aldehyde material in analyte detection process is reduced, improves the order of accuarcy of analysis detection.
Description
Technical field
The present invention relates to a kind of detection method of aldehyde material in processing method of buccal cigarette sample, buccal cigarette, belong to nothing
Flue gas tobacco product chromatography analysis detection technique field.
Background technology
Smoke-free tobacco product is a kind of tobacco product that tobacco consumption is carried out by non-burning approach, its species is very much,
Wherein the product of in the market mainstream is buccal cigarette.Buccal cigarette refers to the smoke-free tobacco product shape consumed by mouth containing mode
Formula, mainly there is two classes, i.e. Sweden contains cigarette (Snus) and American (Moist snuff) containing cigarette.Sweden is that one kind has Sweden containing cigarette
The wet tobacco powder of style, usually mixes suitable fragrance matter, flavouring, water, humectation by the tobacco powder with certain granules degree
Agent and acid-base modifier is thermally treated is processed into.Moisture has in bulk and two kinds packed generally between 30%~60%
Type.This kind of product is one of ancient smoke-free tobacco product in Northern Europe, most commonly seen in Sweden.In use, can directly it take
A certain amount of bulk products or one bag of bagged product are placed between upper lip and gum.The American cigarette that contains is added by air-curing of tobacco leaves or fire-cured tobacco
A kind of moist tobacco powder or Filamentous tobacco product that work forms.Moisture is usually above 40%, there is in bulk and packed two species
Type, is typically to consume between the lip and gum being contained in.It is more welcome in North America and Europe, it is at present in American market share
A kind of maximum smoke-free tobacco product.
Influenced by our times tobacco control campaign, the important development that smoke-free tobacco product is just becoming international Field of Tobacco becomes
Gesture, while market development is rapid, the harmful components in smoke-free tobacco product also receive the concern of consumer.FDA in
Formaldehyde, acetaldehyde and crotonaldehyde were classified as in smoke-free tobacco product harmful and potentially harmful component list in 2012, but at present
All do not reported both at home and abroad for the detection method of these three aldehyde in smoke-free tobacco product.
Formaldehyde, acetaldehyde and crotonaldehyde are all small molecule aldehyde compounds, and volatility and hydrophily are strong, in reverse-phase chromatographic column
Almost without reserve, ionization is difficult, and the material of larger molecular weight is generally transformed into by Derivatization Method, with enhancing
Stability, improves chromatographic isolation effect and quantitative accuracy, sensitivity.Current detection method is that it is used 2,4- bis- mostly
After nitrophenyl hydrazine (DNPH) derivatization enter high performance liquid chromatography-ultraviolet or diode array (HPLC-UV or HPLC-DAD) into
Row detection, this is also method (the CRM No.74 of Carbonyl compounds in the detection main flume that CORESTA recommends
Determination of Selected Carbonyls in Mainstream Cigarette Smoke by High
Performance Liquid Chromatography (HPLC)) and China's tobacco business issue standard method (YC/T
The measure high performance liquid chromatography of 254-2008 main carbonyl compounds in main stream cigarette smoke；YC/T 378-2010 cigarette is surveyed
Flow the measure high performance liquid chromatography of carbonyls in flue gas).In view of sample morphology and the difference of consumption pattern, this method
It is not particularly suited for the detection of formaldehyde in buccal cigarette, acetaldehyde and crotonaldehyde.
In the prior art, Authorization Notice No. is to disclose a kind of use in the Chinese invention patent of CN104950064B
The method of main carbonyl compounds, this method are extracted using acetic acid aqueous solution in UPLC-IE methods measure smoke-free tobacco product
Main carbonyl compounds in smoke-free tobacco product, are then filtered using polyethersulfone millipore filter, then after filtration molten
2,4-dinitrophenylhydrazine solution is added in liquid to perform the derivatization, and after mixing, waits 15min to take appropriate extraction to the reaction was complete
Take liquid to be filtered with organic phase filter membrane, then carry out UPLC analyses.Place before progress UPLC analyses of this method to smokeless tobacco
Reason process is cumbersome, is unfavorable for quickly detecting, and easily causes the loss of tested substance, reduces the order of accuarcy of detection.
The content of the invention
The object of the present invention is to provide a kind of processing method of buccal cigarette sample, it can be achieved that to aldehyde material in buccal cigarette
Quick detection, improves the order of accuarcy of analysis testing result.
Present invention also offers a kind of detection method of aldehyde material in buccal cigarette.
In order to realize the above object technical solution is used by the processing method of the buccal cigarette sample of the present invention：
A kind of processing method of buccal cigarette sample, comprises the following steps：Into buccal cigarette sample add acidic ph modifier,
Derivatization reagent and extractant are uniformly mixed, stratification, take upper organic phase as sample to be tested；Per 1g buccal cigarette samples pair
The volume of extractant should be used as 8~15ml.
The amount of the derivatization reagent added into buccal cigarette will be enough to make the aldehyde material in buccal cigarette sample mixing
Derivative reaction all occurs in journey.Under normal conditions, the amount of the derivatization reagent of addition is aldehyde material is all spread out
The several times of amount needed for biochemical reaction.Amount such as the derivatization reagent of addition is the desired amount of more than 10 times.
The processing method of the buccal cigarette sample of the present invention, acidic ph modifier, derivatization examination are sequentially added into buccal cigarette
Uniformly mixed process is carried out after agent and extractant, mixing, derivative reaction and liquid-liquid extraction can be achieved at the same time, the process is not only
It can speed up and leach the aldehyde material in buccal cigarette, shorten aldehyde material and the time of derivatization reagent reaction in buccal cigarette,
It can also realize that the product after reaction is carried out liquid-liquid extraction enters organic phase, further speeds up the speed of subsequent derivationization reaction at the same time
Rate, shortens the time of analysis detection, reduces loss of the aldehyde material in analyte detection process；Reaction product is in mixed process
Constantly immerse organic phase can constantly promote again in turn derivative reaction progress and aldehyde material from buccal cigarette sample solid
In dissolution, these can substantially increase analysis detection order of accuarcy.
The order that acidic ph modifier, derivatization reagent and extractant are added into buccal cigarette sample is first to add acid pH
Conditioning agent, then adds derivatization reagent, is eventually adding extractant.
The buccal cigarette sample is to place buccal cigarette 1~2 day at 2~6 DEG C, is claimed after then placing 1~2h at room temperature
Restore.By buccal cigarette before 2~6 DEG C are placed, it should be stored in freezing environment.Placed before weighing at 2~6 DEG C and at room temperature
Time cannot be too long, a large amount of losses of the moisture that is otherwise easy to cause in buccal cigarette and volatile materials.For bulk type mouth
Containing cigarette, room temperature is directly weighed after placing.For packed type buccal cigarette, sack also serves as the part of sample and is included in when weighing
Gross mass；Cut off after weighing, packaging bag also serves as a part for buccal cigarette sample.- 20 DEG C will be stored within 1~2 day before such as weighing
Pack sample taking-up, be placed under 4 DEG C of environment, then at room temperature balance 1~2h after weigh.Remaining sample after weighing
Product are again sealed off being put into -20 DEG C of low temperature environment and preserve.
Preferably, adding acidic ph modifier makes the pH of system water phase be 2.0~3.5.
Preferably, the acidic ph modifier is acidic buffer solution.The acidic buffer solution can use ammonium formate
Solution.The pH of the acidic buffer solution is 2.0~3.5.The acidic buffer solution is ammonium formate buffer solution.Ammonium formate delays
Rushing solution can conventionally be prepared, and after ammonium formate such as is dissolved in water, is added formic acid and adjusted pH to setting value.
Prepared ammonium formate buffer solution preserves at room temperature, and the term of validity is 1 month.
Preferably, the volume ratio of the acidic ph modifier of addition and extractant is 30~50:8~15.
The derivatization reagent is 2,4 dinitrophenyl hydrazine (DNPH).The derivatization reagent added into buccal cigarette sample
When, addition is derivatization reagent solution.Acidic ph modifier, derivatization reagent solution and the extraction added into buccal cigarette sample
The volume ratio for taking agent is 30~50:0.5~2:8~15.
The derivatization reagent solution is the acetonitrile solution of 2,4 dinitrophenyl hydrazine.The concentration of the derivatization reagent solution
For 1~5g/L.For every g tobacco samples, it is 0.2~2mL to add the volume that concentration is 1~5g/L derivatization reagents.Derivatization
Reagent solution should be kept in dark place, and be valid for three months.
The process of mixing is exactly to realize test substance dissolution, derivative reaction and derivative reaction product from water phase transfer
To the process of extractant organic phase.Preferably, described to be mixed into supersound process, the time of supersound process is 10~40min.Using
The method of ultrasound is mixed, and can both accelerate mixing and reaction process, while can accelerate Liquid-liquid Extraction Processes, further contracting
Short aldehydes derivative reaction product is by the distribution time between water phase and organic phase.Mix in addition to it can use and be ultrasonically treated,
It can also be carried out by the way of vibrating, be vortexed or rock.
The extractant is organic solvent.It is preferential to select the less organic solvent conduct of polarity in order to improve extraction efficiency
Extractant.Preferably, the extractant is isohexane or n-hexane.Using isohexane as extractant to buccal cigarette sample pretreatment
Afterwards, retention time when analysis detection is carried out using liquid chromatograph is shorter, and the toxicity of isohexane is small compared with n-hexane.
Technical solution is used by the detection method of aldehyde material in the buccal cigarette of the present invention：
The detection method of aldehyde material, includes the following steps in a kind of buccal cigarette：Acid pH is added into buccal cigarette sample
Conditioning agent, derivatization reagent and extractant are uniformly mixed, stratification, take upper organic phase then to be treated as sample to be tested
Aldehyde material in sample carries out analysis detection；The volume that the extractant added is corresponded to per 1g buccal cigarettes sample is 8~15ml.
The amount of the derivatization reagent added into buccal cigarette will be enough to make the aldehyde material in buccal cigarette sample mixing
Derivative reaction all occurs in journey.
The detection method of aldehyde material, acidic ph modifier is sequentially added into buccal cigarette, is spread out in the buccal cigarette of the present invention
Uniformly mixed process is carried out after biochemical reagents and extractant, mixing, aldehydes derivative reaction and liquid-liquid extraction can be achieved at the same time,
The process can not only accelerate to leach the aldehyde material in buccal cigarette, and it is anti-to shorten aldehyde material and derivatization reagent in buccal cigarette
The time answered, while can also realize that the product after reaction is carried out liquid-liquid extraction enters organic phase, further speeds up subsequent derivation
Change the speed of reaction, shorten the time of analysis detection, reduce loss of the aldehyde material in analyte detection process；Reaction product exists
Constantly immersed in mixed process organic phase can constantly promote again in turn derivative reaction progress and aldehyde material from mouth containing
Dissolution in cigarette sample solid, these all substantially increase the order of accuarcy of analysis detection.Aldehydes in the buccal cigarette of the present invention
The detection method of matter, simple, quick, measurement result is sensitive and accurate, can provide technical support for buccal cigarette control of product quality.
The order that acidic ph modifier, derivatization reagent and extractant are added into buccal cigarette sample is first to add acid pH
Conditioning agent, then adds derivatization reagent, is eventually adding extractant.
The buccal cigarette sample is to place buccal cigarette 1~2 day at 2~6 DEG C, is claimed after then placing 1~2h at room temperature
Restore.For packed type buccal cigarette, sack also serves as the part of sample and is included in gross mass when weighing；Cut off, wrap after weighing
Pack also serves as a part for buccal cigarette sample.The sample that packs for being stored in -20 DEG C was taken out in 1~2 day before such as weighing,
It is placed under 4 DEG C of environment, weighs after then balancing 1~2h at room temperature.Remaining sample after weighing is again sealed off being put into -20
DEG C low temperature environment in preserve.For bulk type buccal cigarette, room temperature is directly weighed after placing.
Preferably, the acidic ph modifier of addition makes the pH of system water phase be 2.0~3.5.
Preferably, the acidic ph modifier is acidic buffer solution.The acidic buffer solution can use ammonium formate
Solution.The pH of the acidic buffer solution is 2.0~3.5.The acidic ph modifier of addition and the volume ratio of extractant for 30~
50:8~15.
The derivatization reagent is 2,4 dinitrophenyl hydrazine.When derivatization reagent is added into buccal cigarette sample, addition
It is derivatization reagent solution.The derivatization reagent solution is the acetonitrile solution of 2,4 dinitrophenyl hydrazine.The derivatization reagent
The concentration of solution is 1~5g/L.
Described to be mixed into supersound process, the time of supersound process is 10~40min.
The extractant is isohexane or n-hexane.
Preferably, the method that the aldehyde material in sample to be tested detects is included carrying out liquid chromatogram using liquid chromatograph
Analysis；Liquid-phase chromatographic analysis uses internal standard method, and internal standard compound is made of the deuterated aldehyde material of the derivatization reagent derivatization.Deuterium
It can be made choice for the composition of aldehyde material according to the species of aldehyde material to be detected, can be a certain aldehydes
The combination of matter or several aldehyde materials.
When being analyzed using internal standard method, during handling buccal cigarette sample, except in buccal cigarette sample
Outside middle addition acidic ph modifier, derivatization reagent and extractant, inner mark solution is also added.
When carrying out liquid-phase chromatographic analysis using internal standard method, series standard sample to be tested matches somebody with somebody used by drafting standard curve
Method processed, comprises the following steps：Acidic buffer solution, standard working solution, inner mark solution, derivatization reagent and extractant are mixed
Uniformly, stratification, takes upper organic phase to obtain series standard sample to be tested as standard sample to be tested.The standard work
Make the series standard solution that liquid is aldehyde material to be measured.Same aldehyde material to be measured is formed necessarily in series standard working solution
Concentration gradient.When such as aldehyde material to be measured is formaldehyde, acetaldehyde and crotonaldehyde, formaldehyde, acetaldehyde and crotonaldehyde in standard working solution
Concentration can use the concentration listed in table 1.
The concentration of formaldehyde, acetaldehyde and crotonaldehyde in 1 standard working solution of table
| Numbering | 1# | 2# | 3# | 4# | 5# | 6# | 7# |
| Formaldehyde (mg/mL) | 0.0001 | 0.0005 | 0.001 | 0.002 | 0.006 | 0.01 | 0.02 |
| Acetaldehyde (mg/mL) | 0.0001 | 0.0005 | 0.001 | 0.002 | 0.006 | 0.01 | 0.02 |
| Crotonaldehyde (mg/mL) | 0.00001 | 0.00005 | 0.0001 | 0.0002 | 0.0006 | 0.001 | 0.002 |
Standard working solution should be prepared before use.
Preferably, the internal standard compound is by formaldehyde-d2-DNPH, acetaldehyde-d4-DNPH and crotonaldehyde -3,5,6-d3-DNPH groups
Into.Detection to formaldehyde, acetaldehyde and crotons aldehyde in buccal cigarette can be realized using the internal standard compound.In the inner mark solution,
The concentration of formaldehyde-d2-DNPH is 0.1mg/mL, and the concentration of acetaldehyde-d4-DNPH is 0.1mg/mL, crotonaldehyde -3,5,6-d3-
The concentration of DNPH is 0.01mg/mL.When formaldehyde, acetaldehyde and crotonaldehyde in buccal cigarette carry out analysis detection, can also use
Other deuterated things of formaldehyde, acetaldehyde and crotonaldehyde use the compound obtained after derivatization reagent derivatization as internal standard compound.
Analysis detection is carried out to the aldehyde material in sample to be tested can use liquid chromatograph mass spectrography.Using liquid phase
During chromatograph-mass spectrometer coupling, with the molecular ion peak of aldehyde material to be measured in standard sample to be tested and corresponding deuterated aldehyde material
Molecular ion peak area ratio is response signal (y), to concentration (x) of the aldehyde material to be measured in standard sample to be tested into line
Property fitting, obtain standard curve.Carry out that during linear fit least square method can be used, the weight of concentration (x) is 1/x.Mouth containing
The aldehyde material to be measured that the content of aldehyde material to be measured can be in sample to be tested in cigarette sample and corresponding deuterated aldehyde material
The ratio between integral area and standard curve be calculated.
The liquid-phase chromatographic analysis includes following chromatographic condition：Column temperature is 20~30 DEG C；Mobile phase A is ultra-pure water, stream
Dynamic phase B is acetonitrile, gradient elution.The resistivity for the ultra-pure water that mobile phase A uses is 18.20M Ω cm.What Mobile phase B used
Acetonitrile is chromatographically pure.The temperature of sample room is 3~5 DEG C.The volume of sample introduction is 1~10 μ L.
The chromatographic column that liquid-phase chromatographic analysis can use is C18 chromatographic columns or C8 chromatographic column.Using the C8 colors of same size
The appearance of column is composed compared with C18 chromatographic columns evening.
Preferably, the liquid-phase chromatographic analysis is analyzed for ultra performance liquid chromatography.Mainly may be used using ultra performance liquid chromatography
To shorten retention time.The internal diameter of C18 chromatographic columns that ultra performance liquid chromatography analysis uses for 2.1mm, length be 50mm or
100mm, the particle diameter of filler is 1.7 μm.When carrying out ultra performance liquid chromatography analysis using above-mentioned C18 chromatographic columns, mobile phase
Flow velocity is 0.4~0.5mL/min.
The gradient that the ultra performance liquid chromatography analysis uses is as shown in table 2.
2 gradient table of table
| Time (min) | Mobile phase A (%) | Mobile phase B (%) | Gradient curve |
| 0 | 45 | 55 | Linearly |
| 0.2 | 45 | 55 | Linearly |
| 1.0 | 0 | 100 | Linearly |
| 1.5 | 0 | 100 | Linearly |
| 1.8 | 45 | 55 | Linearly |
| 4.1 | 45 | 55 | Linearly |
When progress liquid chromatograph mass spectrography carries out analysis detection, the mass spectrograph used can be arbitrary high-resolution
Mass spectrograph, such as uses Q-Exactive type high-resolution mass spectrometers.When being analyzed using high-resolution mass spectrometer, Mass Spectrometry Conditions bag
Include：Electrical heating esi ion source (HESI)；300 DEG C of ion source heating temperature；Negative ion mode；It is sheath gas (Sheath gas), auxiliary
It is respectively 30,10 and 0arb to help gas (Aux gas) and purge gass (Sweep gas) flow velocity；Spray voltage 2.5kV；Ion transmits
320 DEG C of capillary heating temperature；Scan pattern target-SIM；Resolution ratio 35000.
Preferably, the analysis detection to the aldehyde material in sample to be tested uses ultra performance liquid chromatography-high resolution mass spectrum
It is combined (UPLC-HRMS).It can be achieved using ultra performance liquid chromatography-high resolution mass spectrum combination fast to aldehyde material in buccal cigarette
Speed, carry out analysis detection exactly.
Brief description of the drawings
Fig. 1 is the selection chromatography of ions figure of 1 Plays sample to be tested of embodiment；
Fig. 2 is the selection chromatography of ions figure of the sample to be tested in embodiment 1.
Embodiment
Technical scheme is further described below in conjunction with embodiment.
The Ultra Performance Liquid Chromatography instrument used in embodiment is 3000 liquid chromatographs of Ultimate, chromatographic column
For ACQUITY UPLC@BEH C18 chromatographic columns (2.1 × 100mm, 1.7 μm, Waters companies)；The high-resolution mass spectrometer of use
For Q-Exactive type high-resolution mass spectrometers.Used formaldehyde-d2-DNPH, acetaldehyde-d4-DNPH and crotonaldehyde -3,5,6-
D3-DNPH is purchased from CDN isotopes.
Embodiment 1
The detection method of aldehyde material in the buccal cigarette of the present embodiment, to the formaldehyde in buccal cigarette, acetaldehyde and crotonaldehyde into
Row analysis detection and analysis, include the following steps：
1) preparation of various solution
1.1) preparation of derivatization reagent solution
0.3g DNPH are weighed, is dissolved with acetonitrile and is settled to 100mL, obtain derivatization reagent solution；Room temperature lucifuge is protected
Deposit, be valid for three months；
1.2) preparation of ammonium formate buffer solution
6.3g ammonium formates are weighed, with about 900mL deionized water dissolvings, first acid for adjusting pH is added to 3.0, then uses deionization
Water is settled to 1L, up to ammonium formate buffer solution；Room temperature preservation, the term of validity are 1 month；
1.3) preparation of series standard working solution includes the following steps：
1.3.1) prepare standard reserving solution
About 50mL deionized waters are added into 100mL volumetric flasks, 100mg formaldehyde is added, is determined after mixing with deionized water
Hold, obtain formalin；Same method prepares acetaldehyde solution and crotonaldehyde solution；Then taken respectively according to actual concentrations certain
Volume mixture and with deionized water constant volume, obtains the mixing of 0.1mg/mL formaldehyde, 0.1mg/mL acetaldehyde and 0.01mg/mL crotonaldehydes
Solution, as standard reserving solution；For standard reserving solution in 4 DEG C of preservations, the term of validity is 1 month；
1.3.2) the preparation of primary standard solution
1mL standard reserving solutions accurately are pipetted into 10mL volumetric flasks, are settled to scale with deionized water, are obtained primary standard
Solution；For primary standard solution in 4 DEG C of preservations, the term of validity is 1 month；
1.3.3 series standard working solution) is prepared
Accurately pipette 0.1 respectively, 0.5,1mL primary standard solution, 0.2,0.6,1,2mL standard reserving solutions to 10mL capacity
In bottle, scale is settled to deionized water, obtains series standard working solution；This includes the series standard work of 7 standard working solutions
Making solution should prepare before use；
1.4) preparation of inner mark solution
According to 1.3.1) method prepare formaldehyde-d2-DNPH, acetaldehyde-d4-DNPH and crotonaldehyde -3,5,6-d3- respectively
DNPH solution, takes certain volume to mix and uses deionized water constant volume, obtain 0.1mg/mL formaldehyde-d2- respectively according to actual concentrations
DNPH, 0.1mg/mL acetaldehyde-d4-DNPH and 0.01mg/mL crotonaldehyde -3,5, the mixed solution of 6-d3-DNPH are molten as internal standard
Liquid；Inner mark solution is preserved at 4 DEG C, is valid for three months；
2) preparation of sample to be tested and series standard sample to be tested
2.1) buccal cigarette samples weighing
Certain bulk type buccal cigarette that -20 DEG C are placed on after sealing is taken out, places 2 days at 4 DEG C, then puts at room temperature
1h is put, 1g is finally weighed again and is put into as buccal cigarette sample in the conical flask of 50mL；
2.2) preparation of sample to be tested
40mL ammonium formates buffer solution, 0.1mL inner mark solutions, 1mL are sequentially added in buccal cigarette sample into conical flask
Derivatization reagent solution, 10mL isohexanes, are ultrasonically treated 20min, then stratification after sealing, take 1mL upper organic phases to turn
Move in brown sample bottle, as sample to be tested；Sample to be tested carries out subsequent analysis detection in 24h；
2.3) preparation of series standard sample to be tested
40mL Ammonium formate buffers are added in the 50mL conical flasks for being 1~7# to numbering, then respectively in 1~7# tapers
Bottle in respectively add a step 1.3.3) in prepare 1mL standard working solution (7 standard working solutions are used), then
0.1mL inner mark solutions, 1mL derivatization reagents solution, 10mL isohexanes are added in 1~7# conical flasks, is ultrasonically treated after sealing
20min, then stratification, takes 1mL upper organic phases to be transferred in brown sample bottle, as series standard sample to be tested；System
Row standard sample to be tested carries out subsequent analysis detection in 24h；
3) ultra performance liquid chromatography-high resolution mass spectrum detection
Obtained sample to be tested and series standard quasi- sample to be measured are carried out using ultra performance liquid chromatography-high resolution mass spectrum
Analysis detection；The ultra performance liquid chromatography condition is controlled to be：25 DEG C of column temperature；4 DEG C of sample room temperature；5 μ L of sampling volume；Flow velocity
0.45mL/min；Mobile phase A-ultra-pure water (resistivity is 18.20M Ω cm), Mobile phase B-acetonitrile (chromatographically pure)；Gradient is washed
De-, gradient is shown in Table 2；
The Mass Spectrometry Conditions are controlled to be：Electrical heating esi ion source (HESI)；300 DEG C of ion source heating temperature；Negative ion mode；
Sheath gas (Sheath gas), auxiliary gas (Aux gas) and purge gass (Sweep gas) flow velocity are respectively 30,10 and 0arb；Spraying
Voltage 2.5kV；320 DEG C of ion transfer capillary heating-up temperature；Scan pattern target-SIM；Resolution ratio 35000；Sample to be tested
Fig. 1 and Fig. 2 are seen respectively with the selection chromatography of ions figure of series standard sample；
4) data calculate
Quantified using internal standard method, formaldehyde-d2-DNPH, acetaldehyde-d4-DNPH, crotonaldehyde -3,5,6-d3-DNPH difference
It is formaldehyde-DNPH, acetaldehyde-DNPH, the internal standard compound of crotonaldehyde-DNPH；Respectively with formaldehyde in series standard sample to be tested, acetaldehyde and
The ratio between the molecular ion peak of crotonaldehyde and molecular ion peak integral area of corresponding deuterated aldehyde material are response signal (y), are adopted
Concentration (x, weight 1/x) of the corresponding aldehyde material to be measured in series standard sample to be tested is carried out with least square method linear
Fitting, obtains standard curve；
According to standard curve and to sample to be tested carry out that ultra performance liquid chromatography-high resolution mass spectrum detects as a result, right
The content of aldehyde material to be measured is calculated in buccal cigarette sample.
Embodiment 2
The present embodiment is the detection to the formaldehyde in packed type buccal cigarette, acetaldehyde and crotonaldehyde；Aldehyde material in buccal cigarette
Detection method, in addition to buccal cigarette samples weighing is to follow the steps below, remaining step is completely the same as embodiment 1：
The sample that packs for being stored in -20 DEG C is taken out, takes out a pouch packed type buccal cigarette (the packed type of a pouch
The quality of buccal cigarette is about 1g) placed under 4 DEG C of environment 2 days, weigh after then balancing 2h at room temperature, cut off after weighing,
Tobacco powder is put into the conical flask of 50mL together with packaging bag；Remaining sample is again sealed off being put into -20 DEG C of low temperature ring after packing
In border.
Embodiment 3
The detection method of aldehyde material in the buccal cigarette of the present embodiment, to the formaldehyde in buccal cigarette, acetaldehyde and crotonaldehyde into
Row analysis detection and analysis, include the following steps：
1) preparation of various solution
1.1) preparation of derivatization reagent solution
0.1g DNPH are weighed, is dissolved with acetonitrile and is settled to 100mL, obtain derivatization reagent solution；Room temperature lucifuge is protected
Deposit, be valid for three months；
1.2) preparation of ammonium formate buffer solution
Weigh 0.63g ammonium formates, with about 900mL deionized water dissolvings, add first acid for adjusting pH to 2.5, then spend from
Sub- water is settled to 1L, up to ammonium formate buffer solution；Room temperature preservation, the term of validity are 1 month；
1.3) preparation of series standard working solution includes the following steps：
1.3.1) prepare standard reserving solution
About 50mL deionized waters are added into 100mL volumetric flasks, 100mg formaldehyde is added, is determined after mixing with deionized water
Hold, obtain formalin；Same method prepares acetaldehyde solution and crotonaldehyde solution；Then taken respectively according to actual concentrations certain
Volume mixture and with deionized water constant volume, obtains the mixing of 0.1mg/mL formaldehyde, 0.1mg/mL acetaldehyde and 0.01mg/mL crotonaldehydes
Solution, as standard reserving solution；For standard reserving solution in 4 DEG C of preservations, the term of validity is 1 month；
1.3.2) the preparation of primary standard solution
1mL standard reserving solutions accurately are pipetted into 10mL volumetric flasks, are settled to scale with deionized water, are obtained primary standard
Solution；For primary standard solution in 4 DEG C of preservations, the term of validity is 1 month；
1.3.3 series standard working solution) is prepared
Accurately pipette 0.1 respectively, 0.5,1mL primary standard solution, 0.2,0.6,1,2mL standard reserving solutions to 10mL capacity
In bottle, scale is settled to deionized water, obtains series standard working solution；This includes the series standard work of 7 standard working solutions
Making solution should prepare before use；
1.4) preparation of inner mark solution
According to 1.3.1) method prepare formaldehyde-d2-DNPH, acetaldehyde-d4-DNPH and crotonaldehyde -3,5,6-d3- respectively
DNPH solution, takes certain volume to mix and uses deionized water constant volume, obtain 0.1mg/mL formaldehyde-d2- respectively according to actual concentrations
DNPH, 0.1mg/mL acetaldehyde-d4-DNPH and 0.01mg/mL crotonaldehyde -3,5, the mixed solution of 6-d3-DNPH are molten as internal standard
Liquid；Inner mark solution is preserved at 4 DEG C, is valid for three months；
2) preparation of sample to be tested and series standard sample to be tested
2.1) buccal cigarette samples weighing
Certain bulk type buccal cigarette that -20 DEG C are placed on after sealing is taken out, places 2 days at 4 DEG C, then puts at room temperature
2h is put, 1g is finally weighed and is put into as buccal cigarette sample in the conical flask of 100mL；
2.2) preparation of sample to be tested
50mL ammonium formates buffer solution, 0.1mL inner mark solutions, 3mL are sequentially added in buccal cigarette sample into conical flask
Derivatization reagent solution, 8mL isohexanes, are ultrasonically treated 40min, then stratification after sealing, take 1mL upper organic phases to shift
Into brown sample bottle, as sample to be tested；Sample to be tested carries out subsequent analysis detection in 24h；
2.3) preparation of series standard sample to be tested
50mL Ammonium formate buffers are added in the 100mL conical flasks for being 1~7# to numbering, are then bored respectively in 1~7#
In shape bottle respectively add a step 1.3.3) in prepare 1mL standard working solution (7 standard working solutions are used), then
0.1mL inner mark solutions, 3mL derivatization reagents solution, 8mL isohexanes are added in 1~7# conical flasks, is ultrasonically treated after sealing
40min, then stratification, takes 1mL upper organic phases to be transferred in brown sample bottle, as series standard sample to be tested；System
Row standard sample to be tested carries out subsequent analysis detection in 24h；
3) ultra performance liquid chromatography-high resolution mass spectrum detection
Obtained sample to be tested and series standard quasi- sample to be measured are carried out using ultra performance liquid chromatography-high resolution mass spectrum
Analysis detection；The ultra performance liquid chromatography condition is controlled to be：20 DEG C of column temperature；4 DEG C of sample room temperature；4 μ L of sampling volume；Flow velocity
0.4mL/min；Mobile phase A-ultra-pure water (resistivity is 18.20M Ω cm), Mobile phase B-acetonitrile (chromatographically pure)；Gradient elution,
Gradient is shown in Table 2；
The high resolution mass spectrum condition is controlled to be：Electrical heating esi ion source (HESI)；300 DEG C of ion source heating temperature；Bear from
Subpattern；Sheath gas (Sheath gas), auxiliary gas (Aux gas) and purge gass (Sweep gas) flow velocity are respectively 30,10 and
0arb；Spray voltage 2.5kV；320 DEG C of ion transfer capillary heating-up temperature；Scan pattern target-SIM；Resolution ratio
35000；
4) data calculate
Quantified using internal standard method, formaldehyde-d2-DNPH, acetaldehyde-d4-DNPH, crotonaldehyde -3,5,6-d3-DNPH difference
It is formaldehyde-DNPH, acetaldehyde-DNPH, the internal standard compound of crotonaldehyde-DNPH；Respectively with formaldehyde in series standard sample to be tested, acetaldehyde and
The ratio between the molecular ion peak of crotonaldehyde and molecular ion peak integral area of corresponding deuterated aldehyde material are response signal (y), are adopted
Concentration (x, weight 1/x) of the corresponding aldehyde material to be measured in series standard sample to be tested is carried out with least square method linear
Fitting, obtains standard curve；
According to standard curve and to sample to be tested carry out that ultra performance liquid chromatography-high resolution mass spectrum detects as a result, right
The content of aldehyde material to be measured is calculated in buccal cigarette sample.
Embodiment 4
The detection method of aldehyde material in the buccal cigarette of the present embodiment, to the formaldehyde in buccal cigarette, acetaldehyde and crotonaldehyde into
Row analysis detection and analysis, include the following steps：
1) preparation of various solution
1.1) preparation of derivatization reagent solution
0.5g DNPH are weighed, is dissolved with acetonitrile and is settled to 100mL, obtain derivatization reagent solution；Room temperature lucifuge is protected
Deposit, be valid for three months；
1.2) preparation of ammonium formate buffer solution
3.2g ammonium formates are weighed, with about 900mL deionized water dissolvings, first acid for adjusting pH is added to 3.0, then uses deionization
Water is settled to 1L, up to ammonium formate buffer solution；Room temperature preservation, the term of validity are 1 month；
1.3) preparation of series standard working solution includes the following steps：
1.3.1) prepare standard reserving solution
About 50mL deionized waters are added into 100mL volumetric flasks, 100mg formaldehyde is added, is determined after mixing with deionized water
Hold, obtain formalin；Same method prepares acetaldehyde solution and crotonaldehyde solution；Then taken respectively according to actual concentrations certain
Volume mixture and with deionized water constant volume, obtains the mixing of 0.1mg/mL formaldehyde, 0.1mg/mL acetaldehyde and 0.01mg/mL crotonaldehydes
Solution, as standard reserving solution；For standard reserving solution in 4 DEG C of preservations, the term of validity is 1 month；
1.3.2) the preparation of primary standard solution
1mL standard reserving solutions accurately are pipetted into 10mL volumetric flasks, are settled to scale with deionized water, are obtained primary standard
Solution；For primary standard solution in 4 DEG C of preservations, the term of validity is 1 month；
1.3.3 series standard working solution) is prepared
Accurately pipette 0.1 respectively, 0.5,1mL primary standard solution, 0.2,0.6,1,2mL standard reserving solutions to 10mL capacity
In bottle, scale is settled to deionized water, obtains series standard working solution；This includes the series standard work of 7 standard working solutions
Making solution should prepare before use；
1.4) preparation of inner mark solution
According to 1.3.1) method prepare formaldehyde-d2-DNPH, acetaldehyde-d4-DNPH and crotonaldehyde -3,5,6-d3- respectively
DNPH solution, takes certain volume to mix and uses deionized water constant volume, obtain 0.1mg/mL formaldehyde-d2- respectively according to actual concentrations
DNPH, 0.1mg/mL acetaldehyde-d4-DNPH and 0.01mg/mL crotonaldehyde -3,5, the mixed solution of 6-d3-DNPH are molten as internal standard
Liquid；Inner mark solution is preserved at 4 DEG C, is valid for three months；
2) preparation of sample to be tested and series standard sample to be tested
2.1) buccal cigarette samples weighing
The sample that packs for being stored in -20 DEG C is taken out, takes out a pouch packed type buccal cigarette (the packed type of a pouch
The quality of buccal cigarette is about 1g) placed under 4 DEG C of environment 2 days, weigh after then balancing 2h at room temperature, cut off after weighing,
Tobacco powder is put into the conical flask of 50mL together with packaging bag；Remaining sample is again sealed off being put into -20 DEG C of low temperature ring after packing
In border；
2.2) preparation of sample to be tested
30mL ammonium formates buffer solution, 0.1mL inner mark solutions, 1mL are sequentially added in buccal cigarette sample into conical flask
Derivatization reagent solution, 15mL isohexanes, are ultrasonically treated 10min, then stratification after sealing, take 1mL upper organic phases to turn
Move in brown sample bottle, as sample to be tested；Sample to be tested carries out subsequent analysis detection in 24h；
2.3) preparation of series standard sample to be tested
30mL Ammonium formate buffers are added in the 50mL conical flasks for being 1~7# to numbering, then respectively in 1~7# tapers
Bottle in respectively add a step 1.3.3) in prepare 1mL standard working solution (7 standard working solutions are used), then
0.1mL inner mark solutions, 1mL derivatization reagents solution, 15mL isohexanes are added in 1~7# conical flasks, is ultrasonically treated after sealing
10min, then stratification, takes 1mL upper organic phases to be transferred in brown sample bottle, as series standard sample to be tested；System
Row standard sample to be tested carries out subsequent analysis detection in 24h；
3) ultra performance liquid chromatography-high resolution mass spectrum detection
Obtained sample to be tested and series standard quasi- sample to be measured are carried out using ultra performance liquid chromatography-high resolution mass spectrum
Analysis detection；The ultra performance liquid chromatography condition is controlled to be：30 DEG C of column temperature；4 DEG C of sample room temperature；6 μ L of sampling volume；Flow velocity
0.5mL/min；Mobile phase A-ultra-pure water (resistivity is 18.20M Ω cm), Mobile phase B-acetonitrile (chromatographically pure)；Gradient elution,
Gradient is shown in Table 2；
The high-resolution Mass Spectrometry Conditions are controlled to be：Electrical heating esi ion source (HESI)；300 DEG C of ion source heating temperature；It is negative
Ion mode；Sheath gas (Sheath gas), auxiliary gas (Aux gas) and purge gass (Sweep gas) flow velocity are respectively 30,10 and
0arb；Spray voltage 2.5kV；320 DEG C of ion transfer capillary heating-up temperature；Scan pattern target-SIM；Resolution ratio
35000；
4) data calculate
Quantified using internal standard method, formaldehyde-d2-DNPH, acetaldehyde-d4-DNPH, crotonaldehyde -3,5,6-d3-DNPH difference
It is formaldehyde-DNPH, acetaldehyde-DNPH, the internal standard compound of crotonaldehyde-DNPH；Respectively with formaldehyde in series standard sample to be tested, acetaldehyde and
The ratio between the molecular ion peak of crotonaldehyde and molecular ion peak integral area of corresponding deuterated aldehyde material are response signal (y), are adopted
Concentration (x, weight 1/x) of the corresponding aldehyde material to be measured in series standard sample to be tested is carried out with least square method linear
Fitting, obtains standard curve；
According to standard curve and to sample to be tested carry out that ultra performance liquid chromatography-high resolution mass spectrum detects as a result, right
The content of aldehyde material to be measured is calculated in buccal cigarette sample.
Step 2.2) in the present embodiment 1 when preparing sample to be tested, can only into the buccal cigarette sample of conical flask according to
Secondary addition 40mL ammonium formates buffer solution, 1mL derivatization reagents solution, 10mL isohexanes, are ultrasonically treated 20min, so after sealing
Stratification afterwards, takes 1mL upper organic phases to be transferred in brown sample bottle, as sample to be tested.
The sample to be tested obtained for being added without inner mark solution, can also use external standard method to the aldehydes in buccal cigarette sample
Material carries out analysis detection.Since the factors such as the volatility of solvent, the stability of product, the accuracy of sample introduction are to analysis result
Influence very big, during using external standard method, above-mentioned factor is difficult to control, in order to obtain more accurately testing result, generally without considering adopting
Use external standard method.
Experimental example 1
The minimum standard working solution of concentration in step 1.3.3 in embodiment 1 is subjected to ultra performance liquid chromatography-high-resolution matter
Compose (UPLC-HRMS) analysis and test limit (LOD) is calculated with three times signal-to-noise ratio (S/N=3), test limit is in 1.4-3.1ng/mL；Into
Row recovery of standard addition is tested, and parallel determination 5 times, results are averaged (being shown in Table 3).The result shows that the rate of recovery scope of three kinds of aldehyde
Between 100.7%~104.4%, average relative standard's deviation (RSD) is less than 10%.
The analytical performance parameter of 3 formaldehyde of table, acetaldehyde and crotonaldehyde
Experimental example 2
The content of the formaldehyde in certain bulk type buccal cigarette sample, acetaldehyde and crotonaldehyde is repeated using the method for embodiment 1
Measure 5 times, calculates relative standard deviation, obtains method precision, the results are shown in Table 4.
The precision of the detection method of 4 embodiment 1 of table
Note：N.D. it is not detect.
Experimental example 3
The content of the formaldehyde in certain bulk type buccal cigarette sample, acetaldehyde and crotonaldehyde is repeated using the method for embodiment 3
Measure 5 times, calculates relative standard deviation, obtains method precision, the results are shown in Table 5.
The precision of the detection method of 5 embodiment 3 of table
Note：N.D. it is not detect.
Experimental example 4
The content of the formaldehyde in packed type buccal cigarette sample, acetaldehyde and crotonaldehyde is repeated to survey using the method for embodiment 4
It is 5 times fixed, relative standard deviation is calculated, method precision is obtained, the results are shown in Table 6.
The precision of the detection method of 6 embodiment 4 of table
Note：N.D. it is not detect.
Claims (10)
- A kind of 1. processing method of buccal cigarette sample, it is characterised in that：Include the following steps：Added into buccal cigarette sample acid PH adjusting agent, derivatization reagent and extractant are uniformly mixed, stratification, take upper organic phase as sample to be tested；Per 1g mouthfuls The correspondence of sample containing cigarette uses the volume of extractant as 8~15ml.
- 2. the processing method of buccal cigarette sample according to claim 1, it is characterised in that：Acid is added into buccal cigarette sample The order of property pH adjusting agent, derivatization reagent and extractant is first to add acidic ph modifier, then adds derivatization reagent, most After add extractant.
- 3. the processing method of buccal cigarette sample according to claim 1 or 2, it is characterised in that：The buccal cigarette sample is Buccal cigarette is placed 1~2 day at 2~6 DEG C, weighs to obtain after then placing 1~2h at room temperature.
- 4. the processing method of buccal cigarette sample according to claim 1, it is characterised in that：Adding acidic ph modifier makes body The pH for being water phase is 2.0~3.5.
- 5. the processing method of buccal cigarette sample according to claim 1, it is characterised in that：The acidic ph modifier of addition and The volume ratio of extractant is 30~50:8~15.
- 6. the processing method of buccal cigarette sample according to claim 1, it is characterised in that：The extractant for isohexane or N-hexane.
- A kind of 7. detection method of aldehyde material in buccal cigarette, it is characterised in that：Include the following steps：Add into buccal cigarette sample Enter acidic ph modifier, derivatization reagent and extractant to be uniformly mixed, stratification, take upper organic phase as sample to be tested, Then analysis detection is carried out to the aldehyde material in sample to be tested；Often the volume for the extractant that 1g buccal cigarettes sample correspondence adds is 8~15mL.
- 8. the detection method of aldehyde material in buccal cigarette according to claim 7, it is characterised in that：To in sample to be tested The method of aldehyde material detection includes carrying out liquid-phase chromatographic analysis using liquid chromatograph；Liquid-phase chromatographic analysis uses internal standard method, Internal standard compound is made of the deuterated aldehyde material of the derivatization reagent derivatization.
- 9. the detection method of aldehyde material in buccal cigarette according to claim 8, it is characterised in that：The internal standard compound is by first Aldehyde-d2-DNPH, acetaldehyde-d4-DNPH and crotonaldehyde -3,5,6-d3-DNPH compositions.
- 10. the detection method of aldehyde material in buccal cigarette according to claim 8, it is characterised in that：To in sample to be tested Aldehyde material analysis detection using the combination of ultra performance liquid chromatography-high resolution mass spectrum.
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