CN106018635A - Method for pre-processing tobacco or tobacco product and detection method thereof - Google Patents
Method for pre-processing tobacco or tobacco product and detection method thereof Download PDFInfo
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- CN106018635A CN106018635A CN201610658005.2A CN201610658005A CN106018635A CN 106018635 A CN106018635 A CN 106018635A CN 201610658005 A CN201610658005 A CN 201610658005A CN 106018635 A CN106018635 A CN 106018635A
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- Prior art keywords
- dinitrophenylhydrazone
- solution
- carbonyl compound
- aldehyde
- tobacco
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
- G01N30/04—Preparation or injection of sample to be analysed
- G01N30/06—Preparation
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
- G01N30/04—Preparation or injection of sample to be analysed
- G01N30/06—Preparation
- G01N2030/067—Preparation by reaction, e.g. derivatising the sample
Abstract
The invention belongs to the field of detection analysis, and relates to a method for pre-processing tobacco or a tobacco product. The method comprises the following steps: 1) using an acetonitrile extraction tobacco sample or a tobacco product sample to obtain an original extraction solution containing a carbonyl compound; and 2) adding 2,4-dinitrophenylhydrazine and/or 2,4-dinitrophenylhydrazine solution and a strong acid solution in the original extraction solution for derivatization, separating the materials to obtain an extract I containing the carbonyl compound derivatized product. The method also relates to a method for detecting the carbonyl compound in the tobacco or the tobacco product, a kit and a purpose. The method firstly confirms that tobacco and the tobacco product contains the carbonyl compound, the carbonyl compound content in the tobacco or the tobacco product is accurately quantified by the method of the invention, detecting limit is low, sensitivity is high, and repeatability is good.
Description
Technical field
The invention belongs to detect analysis field, be specifically related to a kind of method that Nicotiana tabacum L. or tobacco product are carried out pre-treatment,
Further relate to detect the method for carbonyl compound in Nicotiana tabacum L. or tobacco product.
Background technology
Carbonyl compound is the important harmful components of class in the flue gas that drawing tobacco goods produce, and is put into flue gas 44 kinds
" the Huffman list " of harmful components.This compounds includes formaldehyde, acetaldehyde and acrylic aldehyde etc., and what wherein content was maximum is second
Aldehyde.Low-Molecular-Weight Carbonyl Compounds has stronger ciliary toxicity, and what toxicity was the strongest is low point of acrylic aldehyde, formaldehyde and acetaldehyde etc.
Son amount aldehyde compound, its toxicity increases along with molecular weight and is gradually lowered.Carbonyl compound in flue gas mostlys come from cigarette
The pyrolytic of aldehydes matter in straw-made articles, the aldehydes matter in tobacco product is then to be formed by non enzymatic browning reacton
's.
At present, in main flume, the detection method of carbonyl compound includes: by glass fiber filter trapping main flume
Smoke Particulate, after extraction, carries out quantitative analysis with HPLC-UV detection device.Wherein, extraction uses
Solvent is usually the mixture of organic solvent and water.And, it has been investigated that, the organic solvent ratio in solvent is too high, can lead
The accuracy in detection causing a part of carbonyl compound reduces, and even has some carbonyl compounds to be detected.
Up to now, research worker not yet finds in Nicotiana tabacum L. or tobacco product containing carbonyl compound, also has no to enter it
The detection analysis of row carbonyl compound.
Summary of the invention
The present inventor through lot of experiments it was confirmed containing carbonyl compound in Nicotiana tabacum L. and/or tobacco product.The present invention
People have also obtained a kind of method that Nicotiana tabacum L. or tobacco product are carried out pre-treatment, and the method can be by the carbonyl in Nicotiana tabacum L. or tobacco product
Based compound extracts and is transformed into derivatization product.On this basis, the present inventor be also obtained a kind of detection Nicotiana tabacum L. or
The method of carbonyl compound in tobacco product, is come in Nicotiana tabacum L. or tobacco product by detection carbonyl compound derivatization product
Carbonyl compound carries out detection by quantitative.The accuracy of the method is high, and highly sensitive, detection limit is low, and repeatability is good.
First aspect present invention relates to a kind of method that Nicotiana tabacum L. or tobacco product are carried out pre-treatment, comprises the steps:
(1) with acetonitrile extraction tobacco sample or tobacco product sample, the first extract of carbonyl containing compound is obtained；
(2) in first extract, add 2,4 dinitrophenyl hydrazine and/or 2,4 dinitrophenyl hydrazine solution and strong acid solution enters
Row derivatization, the extracting solution I of isolated carbonyl containing compound derivatization product.
In one embodiment of first aspect present invention, also comprise the steps:
(3) in extracting solution I, add weak base or weak caustic solution, mixing, obtain extracting solution II.
In one embodiment, one or more in pyridine and quinoline of described weak base, preferably pyridine.
In one embodiment, during described weak caustic solution is selected from the acetonitrile solution of pyridine and the acetonitrile solution of quinoline
Plant or multiple, the preferably acetonitrile solution of pyridine.
In one embodiment, the acetonitrile solution (in terms of pyridine) of pyridine or the addition of pyridine are 300-700 μ L/
(mL just extract), preferably 400-600 μ L/ (mL just extract), more preferably 500 μ L/ (mL just extract).
In one embodiment of first aspect present invention, including any one in following A to O or multinomial:
One or more in flammable absorption type smoke straw-made articles and non-combustible absorption type smoke straw-made articles of the most described tobacco product；Excellent
Selection of land, described tobacco product is flammable absorption type smoke straw-made articles, more preferably Medicated cigarette；
The most described carbonyl compound is in formaldehyde, acetaldehyde, acetone, propionic aldehyde, acrylic aldehyde, butyraldehyde, 2-butanone and crotonic aldehyde
One or more；
C., in step (1), the solid-liquid ratio of described extraction is 1:(10-50) (g/mL), preferably 1:(10-30) (g/mL),
More preferably 1:20 (g/mL)；
D., in step (1), described extraction is carried out under oscillating condition；
E. in step (1), extraction time is 10-60 minute, preferably 20-50 minute, more preferably 20 minutes, 30 minutes
Or 50 minutes；
F. in step (1), extraction temperature is room temperature, preferably 5 DEG C-40 DEG C, more preferably 10 DEG C-35 DEG C, the most excellent
Elect 10 DEG C, 25 DEG C or 30 DEG C as；
G. in step (2), 2,4 dinitrophenyl hydrazine solution (in terms of 2,4 dinitrophenyl hydrazine) or 2,4 dinitrophenyl hydrazine
Addition be 0.2-5mg/ (mL just extract), preferably 1-3mg/ (mL just extract), more preferably 2mg/ (mL just extract)；
H., in step (2), the consumption of strong acid solution is 300-700 μ L/ (mL just extract), preferably 400-600 μ L/ (mL
Just extract), more preferably 500 μ L/ (mL just extract)；
I., in step (2), 2,4 dinitrophenyl hydrazine solution is the acetonitrile solution of 2,4 dinitrophenyl hydrazine；Preferably, 2,4-
In the acetonitrile solution of dinitrophenylhydrazine, the concentration of 2,4 dinitrophenyl hydrazine is 1-40mg/mL, more preferably 5-20mg/mL, enters one
Step is preferably 10mg/mL；
J., in step (2), strong acid solution is the acetonitrile solution of strong acid；Preferably, strong acid dense in the acetonitrile solution of strong acid
Degree is 0.05%-2% (W/W), more preferably 0.1%-1% (W/W), more preferably 0.2% (W/W)；
K. in step (2), one or more in perchloric acid solution and hydrofluoric acid solution of strong acid solution；
L. in step (2), the time of derivatization is 20-60 minute, preferably 30-50 minute, more preferably 40 minutes；
M. in step (2), the temperature of derivatization is room temperature, preferably 10 DEG C-35 DEG C；
N., in step (2), carbonyl compound derivatization product is selected from formaldehyde-2,4-dinitrophenylhydrazone, acetaldehyde-2,4-dinitro
Base phenylhydrazone, acetone-2,4-dinitrophenylhydrazone, propionic aldehyde-2,4-dinitrophenylhydrazone, acrylic aldehyde-2,4-dinitrophenylhydrazone, butyraldehyde-2,
One or more in 4-dinitrophenylhydrazone, 2-butanone-2,4-dinitrophenylhydrazone and crotonic aldehyde-2,4-dinitrophenylhydrazone；
O., in step (1), before extraction, the step that tobacco sample or tobacco product sample are carried out to be crushed also is included.
Nicotiana tabacum L. or the pre-treating method of tobacco product described in any one of first aspect present invention are from Nicotiana tabacum L. or Nicotiana tabacum L.
The method separating carbonyl compound in goods.
Second aspect present invention relates to a kind of detecting the method for carbonyl compound in Nicotiana tabacum L. or tobacco product, including according to this
Pre-treating method described in invention any one of first aspect obtains extracting solution I or the step of extracting solution II；Also include using liquid phase color
Spectrum tandem mass spectrometry measures the step of carbonyl compound derivatization product in extracting solution I or extracting solution II.
In one embodiment of second aspect present invention, before being additionally included in liquid chromatography tandem mass spectrometry mensuration, will
Extracting solution I or extracting solution II carry out the step filtered；Preferably, organic facies filter membrane is used to filter；Preferably, organic facies filter
The aperture of film is 0.2-0.6 μm, more preferably 0.45 μm.
In one embodiment of second aspect present invention, described in be determined as detection by quantitative, preferably inner mark method ration inspection
Survey；It is highly preferred that internal standard substance is d3-formaldehyde-2,4 dinitrophenylhydrazone.
In one embodiment of second aspect present invention, it is any that the operating condition of liquid chromatograph includes in following a to d
One or multinomial:
A. chromatographic column is for wearing peace Acclaim Explosive E2 liquid-phase chromatographic column；Preferably, the specification of chromatographic column is
250mm × 4.6mm, 5 μm,
B. the temperature of chromatographic column is 36 DEG C-50 DEG C, preferably 40 DEG C；
C. sample size is 1-10 μ L, preferably 3-7 μ L, more preferably 5 μ L；
D. flowing is made up of mobile phase A and Mobile phase B, and mobile phase A is acetonitrile, and Mobile phase B is water；
Preferably, the elution program of flowing phase is: 0 minute, 60% (V/V) mobile phase A；26 minutes, 60% (V/V) flowed
Phase A；28 minutes, 70% (V/V) mobile phase A；43 minutes, 70% (V/V) mobile phase A；45 minutes, 60% (V/V) mobile phase A,
Remain to the 50th minute；Flow velocity is always 0.6mL/min.
In one embodiment of second aspect present invention, mass spectrographic operating condition or parameter include following 1) to 30) in
Any one or multinomial:
1) ion source is electron spray ionisation source；
2) scan mode is anion scanning；
3) detection mode is multiple-reaction monitoring；
4) electron spray voltage is 3000-6000V, preferably 3500-5000V, more preferably 4500V；
5) ion source temperature is 400 DEG C-650 DEG C, preferably 450 DEG C-550 DEG C, more preferably 500 DEG C；
6) auxiliary gas Gas1 and/or Gas2 pressure be 40-70psi, preferably 50-60psi, more preferably 50psi or
60psi；
7) quota ion of formaldehyde-2,4-dinitrophenylhydrazone is to for 209.0/163.0；
8) the qualitative ion pair of formaldehyde-2,4-dinitrophenylhydrazone is 209.0/151.0；
9) impact energy of formaldehyde-2,4-dinitrophenylhydrazone is-12V；
10) quota ion of acetaldehyde-2,4-dinitrophenylhydrazone is to for 223.0/163.0；
11) the qualitative ion pair of acetaldehyde-2,4-dinitrophenylhydrazone is 223.0/181.0；
12) impact energy of acetaldehyde-2,4-dinitrophenylhydrazone is-16V；
13) quota ion of acetone-2,4-dinitrophenylhydrazone is to for 237.0/207.0；
14) the qualitative ion pair of acetone-2,4-dinitrophenylhydrazone is 237.0/178.0；
15) impact energy of acetone-2,4-dinitrophenylhydrazone is-14V；
16) quota ion of propionic aldehyde-2,4-dinitrophenylhydrazone is to for 237.0/163.0；
17) the qualitative ion pair of propionic aldehyde-2,4-dinitrophenylhydrazone is 237.0/152.0；
18) impact energy of propionic aldehyde-2,4-dinitrophenylhydrazone is-15V；
19) quota ion of acrylic aldehyde-2,4-dinitrophenylhydrazone is to for 235.0/158.0；
20) the qualitative ion pair of acrylic aldehyde-2,4-dinitrophenylhydrazone is 235.0/163.0；
21) impact energy of acrylic aldehyde-2,4-dinitrophenylhydrazone is-16V；
22) quota ion of butyraldehyde-2,4-dinitrophenylhydrazone is to for 251.0/163.0；
23) the qualitative ion pair of butyraldehyde-2,4-dinitrophenylhydrazone is 251.0/152.0；
24) impact energy of butyraldehyde-2,4-dinitrophenylhydrazone is-14V；
25) quota ion of 2-butanone-2,4-dinitrophenylhydrazone is to for 251.0/152.0；
26) the qualitative ion pair of 2-butanone-2,4-dinitrophenylhydrazone is 251.0/163.0；
27) impact energy of 2-butanone-2,4-dinitrophenylhydrazone is-22V；
28) quota ion of crotonic aldehyde-2,4-dinitrophenylhydrazone is to for 249.0/181.0；
29) the qualitative ion pair of crotonic aldehyde-2,4-dinitrophenylhydrazone is 249.0/172.0；
30) impact energy of crotonic aldehyde-2,4-dinitrophenylhydrazone is-18V.
Third aspect present invention relates to a kind of test kit, comprises,
I. acetonitrile；
II.2,4-dinitrophenylhydrazine and/or the acetonitrile solution of 2,4 dinitrophenyl hydrazine；With
III. the acetonitrile solution of perchloric acid.
In one embodiment of third aspect present invention, the acetonitrile that described test kit also comprises pyridine and/or pyridine is molten
Liquid.
In one embodiment of third aspect present invention, described test kit also comprises organic facies filter membrane and d3-formaldehyde-2,
4 dinitrophenylhydrazones.
In one embodiment of third aspect present invention, in the acetonitrile solution of 2,4 dinitrophenyl hydrazine 2,4-dinitro benzene
The concentration of hydrazine is 1-40mg/mL, preferably 5-20mg/mL, more preferably 10mg/mL.
In one embodiment of third aspect present invention, in the acetonitrile solution of perchloric acid, the concentration of perchloric acid is
0.05%-2% (W/W), preferably 0.1%-1% (W/W), more preferably 0.2% (W/W).
Fourth aspect present invention relates to the arbitrary described test kit of third aspect present invention at Nicotiana tabacum L. or the front place of tobacco product
Purposes in reason or the carbonyl compound in detection Nicotiana tabacum L. or tobacco product；Preferably, described tobacco product is selected from flammable
One or more in absorption type smoke straw-made articles and non-combustible absorption type smoke straw-made articles, the most flammable absorption type smoke straw-made articles, further
It is preferably Medicated cigarette.
In one embodiment of fourth aspect present invention, described carbonyl compound selected from formaldehyde, acetaldehyde, acetone, propionic aldehyde,
Any one or more in acrylic aldehyde, butyraldehyde, 2-butanone and crotonic aldehyde.
In the present invention,
If no special instructions, " extraction " refers to utilize suitable solvent and method, by solubility effective ingredient from raw material
The process leached.
If no special instructions, " Nicotiana tabacum L. " refers to Solanaceae, Nicotiana (Nicotiana L.), annual or perennial herb,
Hobby class crop.This genus there are about more than 60 and plants, and is wild species mostly.Main cultispecies has safflower tobacco and Folium Nicotianae rusticae.The two
All originate in South America, be all spontaneous amphidiploid.Safflower tobacco, also known as Nicotiana tabacum, is worldwide commodity production cigarette
Kind.Again because of modulator approach and kind source, area, cultivation step is different and forms polytype: flue-cured tobacco, burley tobaccos, Maryland, snow
Eggplant cigarette, fumigation, Turkish tobaccos, Dark sun-cured, Sun cured tobacco etc..Each type has again a lot of cultivar.Folium Nicotianae rusticae is with the former Soviet Union
Cultivating more with India, there is a small amount of cultivation on the ground such as Xinjiang, China, Gansu.Henbane (N.alata Link and in this genus
Otta) plant for viewing and admiring with powder blue smoke grass (N.glauca Graham).
If no special instructions, " tobacco product " refers to that all or part of is that raw material produces, for suction, suction by Nicotiana tabacum L.
Suck, chew or the goods of snuffing.Described tobacco product includes but not limited to Medicated cigarette and chewing tobacco.
If no special instructions, " flammable absorption type smoke straw-made articles " refers to that smog is lighted and sucked to needs, and smog can be directly sucked in,
Or through filter plug or the filtration of water, it is most commonly that the traditional cigarette of world-wide prevalence.
If no special instructions, " non-combustible absorption type smoke straw-made articles " refers to need not burning, decreases the tar etc. that burning produces
Harmful components, do not produce second-hand flue gas, and adapt to a certain extent and meet consumer's needs to tobacco product, mainly wrap
Include smoke-free tobacco product, Medicated cigarette and electronic cigarette are not burnt in heating.The preparation technology of non-combustible absorption type smoke straw-made articles and combustion absorption type smoke
Straw-made articles has marked difference.
If no special instructions, " carbonyl compound " refers to that the compound containing carbonyl in molecule is referred to as carbonyl compound.
Two representative class carbonyl compounds are 1. aldehyde and ketone, 2. carboxylic acid and derivant thereof.
If no special instructions, " strong acid " refers to the acids that the most almost can all ionize, and has strong acidity anti-
Should, such as hydrochloric acid HCl, sulphuric acid H2SO4, nitric acid HNO3, perchloric acid HCl4Deng.
If no special instructions, " weak base " refer in aqueous can only fraction ionization bases, there is faintly alkaline reaction.
Such as, ammonium hydroxide NH4OH, zinc hydroxide Zn (OH)2, aluminium hydroxide Al (OH)3。
If no special instructions, " internal standard method " refers to draw in Instrumental Analysis a kind of method of standard curve.Its principle is: will
A certain amount of internal standard material adds in the standard solution of variable concentrations level time, and the signal then obtaining composition to be measured and internal standard substance is strong
The ratio of degree, as the longitudinal axis；Obtain the ratio of the amount of composition to be measured or composition to be measured and internal standard substance amount again, as transverse axis, draw and close
It it is curve.Generally, the physics of internal standard material used, chemical property are similar to composition to be measured, and can divide with composition to be measured
From.Internal standard method can eliminate measuring instrument, the change of measuring condition, the impact of sample size change etc., thus improves analysis precision
Degree, is widely used in chromatography and spectrum analysis.
The beneficial effect that the present invention obtains:
1, present invention firstly discovers that containing carbonyl compound in Nicotiana tabacum L., meanwhile, be also to find first tobacco product contains
Carbonyl compound.
2, the pre-treating method of the present invention, can extract the carbonyl compound in Nicotiana tabacum L. or tobacco product and derive
Change.
3, the detection method of the present invention, can go out the carbonyl compound in Nicotiana tabacum L. or tobacco product by accurate quantitative analysis, and detection limit is low,
Highly sensitive, repeatability is good.
4, in detection method, using pure acetonitrile is extraction solvent, and measurable carbonyl compound species is more, accurate
Exactness is higher, and detection limit is lower, and sensitivity is higher.
5, in detection method, liquid chromatograph uses gradient elution, and the chromatographic peak of each carbonyl compound can be made to separate
Du Genggao.
Accompanying drawing explanation
In order to make present disclosure be more likely to be clearly understood, below according to the specific embodiment of the present invention and combine
Accompanying drawing, the present invention is further detailed explanation, wherein
Fig. 1 is that the present invention extracts the flow chart of carbonyl compound in Nicotiana tabacum L. or tobacco product；
Fig. 2 is the reaction equation of carbonyl compound of the present invention and 2,4 dinitrophenyl hydrazine derivative reaction；
Fig. 3 is the chromatogram of S3 grade standard working solution in the embodiment of the present invention 1；
Fig. 4 is the chromatogram of sample solution in the embodiment of the present invention 1；
Fig. 5 is the chromatogram of sample solution in comparative example 2 of the present invention.
Detailed description of the invention
Embodiment 1
1, material and reagent
The standard substance of (1) 8 kind of carbonyl compound-2,4-dinitrophenylhydrazone (buy from lark prestige Science and Technology Ltd.): first
Aldehyde-2,4-dinitrophenylhydrazone, acetaldehyde-2,4-dinitrophenylhydrazone, propionic aldehyde-2,4-dinitrophenylhydrazone, acetone-2,4-dinitro benzene
Hydrazone, acrylic aldehyde-2,4-dinitrophenylhydrazone, butyraldehyde-2,4-dinitrophenylhydrazone, 2-butanone-2,4-dinitrophenylhydrazone and crotonic aldehyde-2,
4-dinitrophenylhydrazone.
(2) internal standard substance d3-formaldehyde-2,4-dinitrophenylhydrazone, buy from lark prestige Science and Technology Ltd..
(3) internal standard storing solution: internal standard substance d3-formaldehyde-2,4-dinitrophenylhydrazone acetontrile becomes concentration to be 50ng/mL's
Internal standard storing solution.
(4) standard working solution: weigh 8 kinds of carbonyl compound-2,4-dinitrophenylhydrazone standard substance and internal standard substance, add second
Nitrile dissolves, and is configured to the 5 grade standard working solutions with Concentraton gradient.Each carbonyl compound-2,4-in 5 grade standard working solutions
The concentration of dinitrophenylhydrazone is as shown in table 1, and internal standard substance concentration is 50ng/mL.
The concentration (ng/mL) of each carbonyl compound-2,4-dinitrophenylhydrazone in table 15 grade standard working solution
| Sequence number | Material | S1 | S2 | S3 | S4 | S5 |
| 1 | Formaldehyde-2,4-dinitrophenylhydrazone | 10.01 | 30.03 | 50.05 | 100.10 | 300.30 |
| 2 | Acetaldehyde-2,4-dinitrophenylhydrazone | 7.43 | 22.30 | 37.16 | 74.33 | 222.98 |
| 3 | Acetone-2,4-dinitrophenylhydrazone | 10.48 | 31.44 | 52.40 | 104.80 | 314.41 |
| 4 | Propionic aldehyde-2,4-dinitrophenylhydrazone | 9.80 | 29.40 | 49.00 | 97.99 | 293.97 |
| 5 | Acrylic aldehyde-2,4-dinitrophenylhydrazone | 4.86 | 14.59 | 24.32 | 48.63 | 145.90 |
| 6 | Butyraldehyde-2,4-dinitrophenylhydrazone | 9.50 | 28.50 | 47.50 | 94.99 | 284.97 |
| 7 | 2-butanone-2,4-dinitrophenylhydrazone | 8.42 | 25.26 | 42.11 | 84.21 | 252.63 |
| 8 | Crotonic aldehyde-2,4-dinitrophenylhydrazone | 9.46 | 28.39 | 47.32 | 94.64 | 283.93 |
In terms of carbonyl compound, the material concentration in 5 grade standard working solutions is as shown in table 2.Internal standard substance concentration is still
50ng/mL.If sample concentration is beyond standard working solution coverage, can suitable extension standards working solution coverage.
Material concentration (ng/mL) in terms of carbonyl compound in table 2 standard working solution
| Sequence number | Material | S1 | S2 | S3 | S4 | S5 |
| 1 | Formaldehyde | 1.43 | 4.29 | 7.15 | 14.30 | 42.90 |
| 2 | Acetaldehyde | 1.46 | 4.38 | 7.30 | 14.60 | 43.80 |
| 3 | Acetone | 2.55 | 7.66 | 12.77 | 25.54 | 76.62 |
| 4 | Propionic aldehyde | 2.39 | 7.16 | 11.94 | 23.88 | 71.64 |
| 5 | Acrylic aldehyde | 1.15 | 3.46 | 5.77 | 11.54 | 34.62 |
| 6 | Butyraldehyde | 2.71 | 8.14 | 13.57 | 27.14 | 81.42 |
| 7 | 2-butanone | 2.41 | 7.22 | 12.03 | 24.06 | 72.18 |
| 8 | Crotonic aldehyde | 2.65 | 7.95 | 13.25 | 26.50 | 79.50 |
2, extract
According to the flow process of Fig. 1, the carbonyl compound in Nicotiana tabacum L. is extracted.
Nicotiana tabacum L. 1 (Yunnan tobacco) is milled to offal, accurately weighs 1g offal sample, be placed in 50mL centrifuge tube, accurately
Adding the vibration extraction of 20mL acetonitrile, extraction temperature is 25 DEG C, and extraction time is 30 minutes；Take the first extract 1mL after extraction in
In 10mL volumetric flask, the acetonitrile solution and the 500 μ L concentration that add the 2,4 dinitrophenyl hydrazine of 200 μ L10mg/mL are 0.2% (W/
The acetonitrile solution of perchloric acid W), mixing, room temperature is placed and within 40 minutes, is performed the derivatization reaction (reaction equation is as shown in Figure 2).
Afterwards, add 500 μ L pyridines and 20 μ L internal standard storing solutions, with acetonitrile constant volume to 10mL, cross 0.45 μm organic facies filter membrane, obtain sample
Product solution.
3, detection
With high performance liquid chromatography tandem mass spectrum instrument (ABSCIEX company Qtrap 5500) respectively to 5 grade standard working solutions
Carry out detection with sample solution to analyze.The chromatogram of S3 grade standard working solution is as shown in Figure 3.The chromatogram of sample solution such as figure
Shown in 4.
Operation condition of chromatogram: chromatographic column uses wears peace Acclaim Explosive E2 liquid-phase chromatographic column, and specification is 250mm
× 4.6mm, 5 μm,Chromatogram column temperature is 40 DEG C；Sample size is 5 μ L；Flowing phase: mobile phase A is acetonitrile, Mobile phase B
For water；The gradient elution program of flowing phase: 0 minute, 60% (V/V) mobile phase A；26 minutes, 60% (V/V) mobile phase A；28 points
Clock, 70% (V/V) mobile phase A；43 minutes, 70% (V/V) mobile phase A；45 minutes, 60% (V/V) mobile phase A；Remain to
50 minutes；Flow velocity is always 0.6mL/min.
Mass spectrum operation condition: ion source: electron spray ionisation source (ESI)；Scan mode: anion scans；Detection mode: many
Reaction monitoring (MRM)；Electron spray voltage: 4500V；Ion source temperature: 500 DEG C；Auxiliary gas Gas1 pressure: 60psi；Auxiliary gas
Gas2 pressure: 50psi.
, qualitative ion pair and collision energy (CE) are shown in Table by the quota ion of each carbonyl compound-2,4-dinitrophenylhydrazone
3。
Table 3 carbonyl compound-2,4-dinitrophenylhydrazone mass spectrometry parameters
4, calculate
(1) according to the testing result of 5 grade standard working solutions in above 3., with carbonyl compound-2,4-dinitrophenylhydrazone
With the peak area ratio of internal standard substance, carbonyl compound-2,4-dinitrophenylhydrazone are carried out linear regression with the concentration ratio of internal standard substance,
To standard curve equation, it is shown in Table 4.Wherein, carbonyl compound-2, the concentration of 4-dinitrophenylhydrazone is with the carbonyl compound in table 2
Densitometer.
In standard curve equation, abscissa represents carbonyl compound-2, and 4-dinitrophenylhydrazone concentration is (dense with carbonyl compound
Degree meter) and internal standard substance concentration proportion, vertical coordinate represents carbonyl compound-2,4-dinitrophenylhydrazone peak area and internal standard substance peak area
Ratio.Taking least concentration standard working solution, 10 parallel assays, calculate standard deviation, 3 times of standard deviations are detection limit, 10
Times standard deviation is quantitative limit, is listed in table 4.
Table 4 standard curve equation, detection limit and quantitative limit
| Object | Equation of linear regression | r | Detection limit (μ g/g) | Quantitative limit (μ g/g) |
| Formaldehyde | Y=0.16x+0.012 | 0.9994 | 0.14 | 0.5 |
| Acetaldehyde | Y=0.18x-0.039 | 0.9998 | 0.14 | 0.5 |
| Acetone | Y=0.23x-0.042 | 0.9995 | 0.26 | 0.9 |
| Propionic aldehyde | Y=0.27x+0.033 | 0.9994 | 0.30 | 1.0 |
| Acrylic aldehyde | Y=0.25x-0.07 | 0.9997 | 0.15 | 0.5 |
| Butyraldehyde | Y=0.29x-0.016 | 0.9996 | 0.30 | 1.0 |
| 2-butanone | Y=0.19x-0.026 | 0.9998 | 0.25 | 0.9 |
| Crotonic aldehyde | Y=0.24x-0.061 | 0.9997 | 0.26 | 0.9 |
(2) according to carbonyl compound-2 in sample solution, the peak area testing result of 4-dinitrophenylhydrazone and internal standard substance, knot
Close the standard curve equation of table 4, be calculated the concentration of carbonyl compound in sample solution, be calculated Nicotiana tabacum L. further according to following formula
The content of middle carbonyl compound, the results are shown in Table 5.
Wherein,
Carbonyl compound content in y Nicotiana tabacum L., μ g/g；
Carbonyl compound concentration in c sample solution, μ g/mL；
V sample solution volume, mL；
M tobacco leaf weight, g.
Embodiment 2
With reference to the method for embodiment 1, the containing of each carbonyl compound in detection Nicotiana tabacum L. 2, Nicotiana tabacum L. 3, Nicotiana tabacum L. 4, Nicotiana tabacum L. 5 respectively
Amount, the results are shown in Table 5.
The content (μ g/g) of carbonyl compound in the different Nicotiana tabacum L. of table 5
| Formaldehyde | Acetaldehyde | Acetone | Propionic aldehyde | Acrylic aldehyde | Butyraldehyde | 2-butanone | Crotonic aldehyde | |
| Nicotiana tabacum L. 1 | 2.33 | 1.46 | 2.26 | 1.03 | LOQ | LOQ | LOQ | LOQ |
| Nicotiana tabacum L. 2 | 2.46 | 1.72 | 1.93 | LOQ | LOQ | LOQ | LOQ | LOQ |
| Nicotiana tabacum L. 3 | 2.98 | 2.06 | 2.85 | 1.24 | LOQ | LOQ | LOQ | LOQ |
| Nicotiana tabacum L. 4 | 3.04 | 2.13 | 2.97 | LOQ | LOQ | LOQ | LOQ | LOQ |
| Nicotiana tabacum L. 5 | 1.96 | 1.43 | 2.31 | LOQ | LOQ | LOQ | LOQ | LOQ |
Note: LOQ represents and does not detects.
As shown in Table 5, the inventive method is relatively low to the detection limit of carbonyl compound, and sensitivity is higher.
Embodiment 3
On the basis of embodiment 1, by 8 kinds of carbonyl compounds respectively with high, medium and low three horizontal mark-ons, each add standard specimen
Product parallel assay is averaged for three times, records the response rate and repeatability (RSD), the results are shown in Table 6.
The response rate of table 6 method and repeatability
As shown in Table 6, the inventive method is to the recovery of standard addition of 8 kinds of carbonyl compounds all more than 92%, and detection is accurately
Degree height, repeatability is good.
Comparative example 1
Respectively with acetonitrile and the volume ratio of water as 1:1 with the mixed solvent of 2:1 replaces pure acetonitrile to extract Nicotiana tabacum L. 1,
Remaining operation is carried out with reference to embodiment 1.
Determine the content of each carbonyl compound in Nicotiana tabacum L. 1 as shown in table 7.
Table 7
Note: LOQ represents and does not detects.
The testing result contrast of Nicotiana tabacum L. 1 in table 7 and table 5 is understood, extract with the mixed solvent of acetonitrile and water compared with, this
When inventive method extracts with pure acetonitrile, the accuracy of detection is higher, and measurable carbonyl compound species is more, and detection limit is lower,
Sensitivity is higher.
Comparative example 2
Using 60% (V/V) acetonitrile+40% (V/V) water to carry out isocratic elution mutually as flowing, remaining operation is with reference to implementing
Example 1 is carried out, and obtains the chromatogram of sample solution as shown in Figure 5.
Comparison diagram 4-5 understand, with 60% (V/V) acetonitrile+40% (V/V) water make flowing equality eluting compared with, this
The chromatographic peak of each carbonyl compound can be separated well by the gradient elution that bright method uses.
Obviously, above-described embodiment is only for clearly demonstrating example, and not restriction to embodiment.Right
For those of ordinary skill in the field, can also make on the basis of the above description other multi-form change or
Variation.Here without also cannot all of embodiment be given exhaustive.And the obvious change thus extended out or
Change among still in the protection domain of the invention.
Claims (10)
1. method Nicotiana tabacum L. or tobacco product being carried out pre-treatment, comprises the steps:
(1) with acetonitrile extraction tobacco sample or tobacco product sample, the first extract of carbonyl containing compound is obtained；
(2) in first extract, add 2,4 dinitrophenyl hydrazine and/or 2,4 dinitrophenyl hydrazine solution and strong acid solution spreads out
Biochemistry, the extracting solution I of isolated carbonyl containing compound derivatization product.
Pre-treating method the most according to claim 1, also comprises the steps,
(3) in extracting solution I, add weak base or weak caustic solution, mixing, obtain extracting solution II；
Preferably, one or more in pyridine and quinoline of described weak base, more preferably pyridine；
Preferably, one or more in the acetonitrile solution of pyridine and the acetonitrile solution of quinoline of described weak caustic solution, more excellent
Elect the acetonitrile solution of pyridine as；
It is highly preferred that the addition of the acetonitrile solution of pyridine (in terms of pyridine) or pyridine is 300-700 μ L/ (mL just extract),
More preferably 400-600 μ L/ (mL just extract), more preferably 500 μ L/ (mL just extract).
Pre-treating method the most according to claim 1 and 2, it is characterised in that any one in following A to O or many
:
One or more in flammable absorption type smoke straw-made articles and non-combustible absorption type smoke straw-made articles of the most described tobacco product；Preferably
Ground, described tobacco product is flammable absorption type smoke straw-made articles, more preferably Medicated cigarette；
The most described carbonyl compound is selected from formaldehyde, acetaldehyde, acetone, propionic aldehyde, acrylic aldehyde, butyraldehyde, 2-butanone and crotonic aldehyde
Plant or multiple；
C., in step (1), the solid-liquid ratio of described extraction is 1:(10-50) (g/mL), preferably 1:(10-30) (g/mL), more excellent
Elect 1:20 (g/mL) as；
D., in step (1), described extraction is carried out under oscillating condition；
E. in step (1), extraction time is 10-60 minute, preferably 20-50 minute, more preferably 20 minutes, 30 minutes or 50
Minute；
F., in step (1), extraction temperature is room temperature, preferably 5-40 DEG C, more preferably 10-35 DEG C, more preferably 10 DEG C,
25 DEG C or 30 DEG C；
G. in step (2), adding of 2,4 dinitrophenyl hydrazine solution (in terms of 2,4 dinitrophenyl hydrazine) or 2,4 dinitrophenyl hydrazine
Dosage is 0.2-5mg/ (mL just extract), preferably 1-3mg/ (mL just extract), more preferably 2mg/ (mL just extract)；
H., in step (2), the consumption of strong acid solution is 300-700 μ L/ (mL just extract), and preferably 400-600 μ L/ (carries at the beginning of mL
Liquid), more preferably 500 μ L/ (mL just extract)；
I., in step (2), 2,4 dinitrophenyl hydrazine solution is the acetonitrile solution of 2,4 dinitrophenyl hydrazine；Preferably, 2,4-dinitros
In the acetonitrile solution of base phenylhydrazine, the concentration of 2,4 dinitrophenyl hydrazine is 1-40mg/mL, more preferably 5-20mg/mL, the most excellent
Elect 10mg/mL as；
J., in step (2), strong acid solution is the acetonitrile solution of strong acid；Preferably, in the acetonitrile solution of strong acid, the concentration of strong acid is
0.05%-2% (W/W), more preferably 0.1%-1% (W/W), more preferably 0.2% (W/W)；
K. in step (2), one or more in perchloric acid solution and hydrofluoric acid solution of strong acid solution；
L. in step (2), the time of derivatization is 20-60 minute, preferably 30-50 minute, more preferably 40 minutes；
M. in step (2), the temperature of derivatization is room temperature, preferably 10 DEG C-35 DEG C；
N., in step (2), carbonyl compound derivatization product is selected from formaldehyde-2,4-dinitrophenylhydrazone, acetaldehyde-2,4-dinitro benzene
Hydrazone, acetone-2,4-dinitrophenylhydrazone, propionic aldehyde-2,4-dinitrophenylhydrazone, acrylic aldehyde-2,4-dinitrophenylhydrazone, butyraldehyde-2,4-two
One or more in nitro phenylhydrazone, 2-butanone-2,4-dinitrophenylhydrazone and crotonic aldehyde-2,4-dinitrophenylhydrazone；
O., in step (1), before extraction, the step that tobacco sample or tobacco product sample are carried out to be pulverized also is included.
4. detect a method for carbonyl compound in Nicotiana tabacum L. or tobacco product, including according to institute any one of claims 1 to 3
The pre-treating method stated obtains extracting solution I or the step of extracting solution II；Also include measuring with liquid chromatography tandem mass spectrometry extracting
The step of carbonyl compound derivatization product in liquid I or extracting solution II；
Alternatively, before being additionally included in liquid chromatography tandem mass spectrometry mensuration, extracting solution I or extracting solution II are carried out the step filtered
Suddenly；Preferably, organic facies filter membrane is used to filter；Preferably, the aperture of organic facies filter membrane is 0.2-0.6 μm, more preferably
0.45μm。
Detection method the most according to claim 4, wherein, described in be determined as detection by quantitative, preferably inner mark method ration inspection
Survey；It is highly preferred that internal standard substance is d3-formaldehyde-2,4 dinitrophenylhydrazone.
6. during according to the detection method described in claim 4 or 5, wherein, the operating condition of liquid chromatograph includes following a to d
Any one or multinomial:
A. chromatographic column is for wearing peace Acclaim Explosive E2 liquid-phase chromatographic column；Preferably, the specification of chromatographic column be 250mm ×
4.6mm, 5 μm,
B. the temperature of chromatographic column is 36 DEG C-50 DEG C, preferably 40 DEG C；
C. sample size is 1-10 μ L, preferably 3-7 μ L, more preferably 5 μ L；
D. flowing is made up of mobile phase A and Mobile phase B, and mobile phase A is acetonitrile, and Mobile phase B is water；
Preferably, the elution program of flowing phase is: 0 minute, 60% (V/V) mobile phase A；26 minutes, 60% (V/V) mobile phase A；
28 minutes, 70% (V/V) mobile phase A；43 minutes, 70% (V/V) mobile phase A；45 minutes, 60% (V/V) mobile phase A, keep
By the 50th minute；Flow velocity is always 0.6mL/min.
7. according to the detection method described in claim 4 or 5, wherein, mass spectrographic operating condition or parameter include following 1) to 30)
In any one or multinomial:
1) ion source is electron spray ionisation source；
2) scan mode is anion scanning；
3) detection mode is multiple-reaction monitoring；
4) electron spray voltage is 3000-6000V, preferably 3500-5000V, more preferably 4500V；
5) ion source temperature is 400 DEG C-650 DEG C, preferably 450 DEG C-550 DEG C, more preferably 500 DEG C；
6) auxiliary gas Gas1 and/or Gas2 pressure are 40-70psi, preferably 50-60psi, more preferably 50psi or 60psi；
7) quota ion of formaldehyde-2,4-dinitrophenylhydrazone is to for 209.0/163.0；
8) the qualitative ion pair of formaldehyde-2,4-dinitrophenylhydrazone is 209.0/151.0；
9) impact energy of formaldehyde-2,4-dinitrophenylhydrazone is-12V；
10) quota ion of acetaldehyde-2,4-dinitrophenylhydrazone is to for 223.0/163.0；
11) the qualitative ion pair of acetaldehyde-2,4-dinitrophenylhydrazone is 223.0/181.0；
12) impact energy of acetaldehyde-2,4-dinitrophenylhydrazone is-16V；
13) quota ion of acetone-2,4-dinitrophenylhydrazone is to for 237.0/207.0；
14) the qualitative ion pair of acetone-2,4-dinitrophenylhydrazone is 237.0/178.0；
15) impact energy of acetone-2,4-dinitrophenylhydrazone is-14V；
16) quota ion of propionic aldehyde-2,4-dinitrophenylhydrazone is to for 237.0/163.0；
17) the qualitative ion pair of propionic aldehyde-2,4-dinitrophenylhydrazone is 237.0/152.0；
18) impact energy of propionic aldehyde-2,4-dinitrophenylhydrazone is-15V；
19) quota ion of acrylic aldehyde-2,4-dinitrophenylhydrazone is to for 235.0/158.0；
20) the qualitative ion pair of acrylic aldehyde-2,4-dinitrophenylhydrazone is 235.0/163.0；
21) impact energy of acrylic aldehyde-2,4-dinitrophenylhydrazone is-16V；
22) quota ion of butyraldehyde-2,4-dinitrophenylhydrazone is to for 251.0/163.0；
23) the qualitative ion pair of butyraldehyde-2,4-dinitrophenylhydrazone is 251.0/152.0；
24) impact energy of butyraldehyde-2,4-dinitrophenylhydrazone is-14V；
25) quota ion of 2-butanone-2,4-dinitrophenylhydrazone is to for 251.0/152.0；
26) the qualitative ion pair of 2-butanone-2,4-dinitrophenylhydrazone is 251.0/163.0；
27) impact energy of 2-butanone-2,4-dinitrophenylhydrazone is-22V；
28) quota ion of crotonic aldehyde-2,4-dinitrophenylhydrazone is to for 249.0/181.0；
29) the qualitative ion pair of crotonic aldehyde-2,4-dinitrophenylhydrazone is 249.0/172.0；
30) impact energy of crotonic aldehyde-2,4-dinitrophenylhydrazone is-18V.
8. a test kit, comprises,
I. acetonitrile；
II.2,4-dinitrophenylhydrazine and/or the acetonitrile solution of 2,4 dinitrophenyl hydrazine；With
III. the acetonitrile solution of perchloric acid；
Preferably, the acetonitrile solution of pyridine and/or pyridine is also comprised；
Preferably, organic facies filter membrane and d are also comprised3-formaldehyde-2,4 dinitrophenylhydrazone；
Preferably, in the acetonitrile solution of 2,4 dinitrophenyl hydrazine, the concentration of 2,4 dinitrophenyl hydrazine is 1-40mg/mL, more preferably
5-20mg/mL, more preferably 10mg/mL；
Preferably, in the acetonitrile solution of perchloric acid, the concentration of perchloric acid is 0.05%-2% (W/W), more preferably 0.1%-1%
(W/W), more preferably 0.2% (W/W).
9. test kit described in claim 8 is in Nicotiana tabacum L. or the pre-treatment of tobacco product or in detection Nicotiana tabacum L. or tobacco product
Purposes in carbonyl compound；Preferably, described tobacco product is selected from flammable absorption type smoke straw-made articles and non-combustible absorption type smoke straw-made articles
In one or more, the most flammable absorption type smoke straw-made articles, more preferably Medicated cigarette.
Purposes the most according to claim 9, wherein, described carbonyl compound selected from formaldehyde, acetaldehyde, acetone, propionic aldehyde, third
Any one or more in olefine aldehydr, butyraldehyde, 2-butanone and crotonic aldehyde.
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