CN111208227A - Method for simultaneously determining content of 8 carbonyl compounds in cigarette blasting beads - Google Patents
Method for simultaneously determining content of 8 carbonyl compounds in cigarette blasting beads Download PDFInfo
- Publication number
- CN111208227A CN111208227A CN202010048812.9A CN202010048812A CN111208227A CN 111208227 A CN111208227 A CN 111208227A CN 202010048812 A CN202010048812 A CN 202010048812A CN 111208227 A CN111208227 A CN 111208227A
- Authority
- CN
- China
- Prior art keywords
- butyraldehyde
- solution
- acetonitrile
- cigarette
- dinitrophenylhydrazone
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
- 235000019504 cigarettes Nutrition 0.000 title claims abstract description 61
- 239000011324 bead Substances 0.000 title claims abstract description 57
- 238000005422 blasting Methods 0.000 title claims abstract description 48
- 238000000034 method Methods 0.000 title claims abstract description 45
- 150000001728 carbonyl compounds Chemical class 0.000 title claims abstract description 30
- WEVYAHXRMPXWCK-UHFFFAOYSA-N Acetonitrile Chemical compound CC#N WEVYAHXRMPXWCK-UHFFFAOYSA-N 0.000 claims abstract description 174
- 239000012488 sample solution Substances 0.000 claims abstract description 34
- 239000003153 chemical reaction reagent Substances 0.000 claims abstract description 28
- 239000012490 blank solution Substances 0.000 claims abstract description 25
- 239000006228 supernatant Substances 0.000 claims abstract description 15
- 238000010812 external standard method Methods 0.000 claims abstract description 10
- 230000010355 oscillation Effects 0.000 claims abstract description 10
- 239000000706 filtrate Substances 0.000 claims abstract description 9
- 238000001914 filtration Methods 0.000 claims abstract description 9
- 239000007788 liquid Substances 0.000 claims abstract description 9
- 239000012528 membrane Substances 0.000 claims abstract description 9
- 239000012074 organic phase Substances 0.000 claims abstract description 9
- ZTQSAGDEMFDKMZ-UHFFFAOYSA-N butyric aldehyde Natural products CCCC=O ZTQSAGDEMFDKMZ-UHFFFAOYSA-N 0.000 claims description 105
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims description 92
- HGINCPLSRVDWNT-UHFFFAOYSA-N Acrolein Chemical compound C=CC=O HGINCPLSRVDWNT-UHFFFAOYSA-N 0.000 claims description 70
- NBBJYMSMWIIQGU-UHFFFAOYSA-N Propionic aldehyde Chemical compound CCC=O NBBJYMSMWIIQGU-UHFFFAOYSA-N 0.000 claims description 70
- 238000001212 derivatisation Methods 0.000 claims description 35
- MLUCVPSAIODCQM-NSCUHMNNSA-N crotonaldehyde Chemical compound C\C=C\C=O MLUCVPSAIODCQM-NSCUHMNNSA-N 0.000 claims description 34
- MLUCVPSAIODCQM-UHFFFAOYSA-N crotonaldehyde Natural products CC=CC=O MLUCVPSAIODCQM-UHFFFAOYSA-N 0.000 claims description 34
- HGBOYTHUEUWSSQ-UHFFFAOYSA-N valeric aldehyde Natural products CCCCC=O HGBOYTHUEUWSSQ-UHFFFAOYSA-N 0.000 claims description 34
- 239000012224 working solution Substances 0.000 claims description 32
- IKHGUXGNUITLKF-XPULMUKRSA-N acetaldehyde Chemical compound [14CH]([14CH3])=O IKHGUXGNUITLKF-XPULMUKRSA-N 0.000 claims description 31
- WSFSSNUMVMOOMR-NJFSPNSNSA-N methanone Chemical compound O=[14CH2] WSFSSNUMVMOOMR-NJFSPNSNSA-N 0.000 claims description 31
- 150000001875 compounds Chemical class 0.000 claims description 30
- 238000002360 preparation method Methods 0.000 claims description 29
- WSFSSNUMVMOOMR-UHFFFAOYSA-N formaldehyde Substances O=C WSFSSNUMVMOOMR-UHFFFAOYSA-N 0.000 claims description 26
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 claims description 20
- 239000012086 standard solution Substances 0.000 claims description 17
- 238000004128 high performance liquid chromatography Methods 0.000 claims description 15
- 239000011550 stock solution Substances 0.000 claims description 15
- IKHGUXGNUITLKF-UHFFFAOYSA-N Acetaldehyde Chemical compound CC=O IKHGUXGNUITLKF-UHFFFAOYSA-N 0.000 claims description 14
- 238000005303 weighing Methods 0.000 claims description 14
- 238000002156 mixing Methods 0.000 claims description 13
- 239000012071 phase Substances 0.000 claims description 12
- 239000000523 sample Substances 0.000 claims description 12
- 238000001514 detection method Methods 0.000 claims description 11
- HORQAOAYAYGIBM-UHFFFAOYSA-N 2,4-dinitrophenylhydrazine Chemical compound NNC1=CC=C([N+]([O-])=O)C=C1[N+]([O-])=O HORQAOAYAYGIBM-UHFFFAOYSA-N 0.000 claims description 10
- 229910000147 aluminium phosphate Inorganic materials 0.000 claims description 10
- 238000010828 elution Methods 0.000 claims description 10
- 238000007865 diluting Methods 0.000 claims description 9
- 239000000243 solution Substances 0.000 claims description 7
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 6
- 239000000919 ceramic Substances 0.000 claims description 5
- 238000011002 quantification Methods 0.000 claims description 5
- JJPZHGIYUVFTGG-UHFFFAOYSA-N 2,4-dinitro-n-(prop-2-enylideneamino)aniline Chemical compound [O-][N+](=O)C1=CC=C(NN=CC=C)C([N+]([O-])=O)=C1 JJPZHGIYUVFTGG-UHFFFAOYSA-N 0.000 claims description 4
- YGIXYAIGWMAGIB-UHFFFAOYSA-N 2,4-dinitro-n-(propan-2-ylideneamino)aniline Chemical compound CC(C)=NNC1=CC=C([N+]([O-])=O)C=C1[N+]([O-])=O YGIXYAIGWMAGIB-UHFFFAOYSA-N 0.000 claims description 4
- 238000006243 chemical reaction Methods 0.000 claims description 4
- 150000007857 hydrazones Chemical class 0.000 claims description 4
- 239000000203 mixture Substances 0.000 claims description 4
- IKGRHEWIFBFXPP-UHFFFAOYSA-N n-(butylideneamino)-2,4-dinitroaniline Chemical compound CCCC=NNC1=CC=C([N+]([O-])=O)C=C1[N+]([O-])=O IKGRHEWIFBFXPP-UHFFFAOYSA-N 0.000 claims description 4
- ONBOQRNOMHHDFB-UHFFFAOYSA-N n-(ethylideneamino)-2,4-dinitroaniline Chemical compound CC=NNC1=CC=C([N+]([O-])=O)C=C1[N+]([O-])=O ONBOQRNOMHHDFB-UHFFFAOYSA-N 0.000 claims description 4
- UEQLSLWCHGLSML-UHFFFAOYSA-N n-(methylideneamino)-2,4-dinitroaniline Chemical compound [O-][N+](=O)C1=CC=C(NN=C)C([N+]([O-])=O)=C1 UEQLSLWCHGLSML-UHFFFAOYSA-N 0.000 claims description 4
- NFQHZOZOFGDSIN-UHFFFAOYSA-N 2,4-dinitro-n-(propylideneamino)aniline Chemical compound CCC=NNC1=CC=C([N+]([O-])=O)C=C1[N+]([O-])=O NFQHZOZOFGDSIN-UHFFFAOYSA-N 0.000 claims description 3
- 239000012295 chemical reaction liquid Substances 0.000 claims description 3
- 238000011084 recovery Methods 0.000 abstract description 10
- 239000000047 product Substances 0.000 abstract description 8
- 238000000926 separation method Methods 0.000 abstract description 4
- 239000000463 material Substances 0.000 abstract description 3
- 230000000694 effects Effects 0.000 abstract description 2
- 238000007689 inspection Methods 0.000 abstract description 2
- 230000035945 sensitivity Effects 0.000 abstract description 2
- 239000000126 substance Substances 0.000 abstract description 2
- 238000000605 extraction Methods 0.000 abstract 1
- 238000004587 chromatography analysis Methods 0.000 description 7
- 238000004458 analytical method Methods 0.000 description 4
- 230000000391 smoking effect Effects 0.000 description 4
- 238000010586 diagram Methods 0.000 description 3
- 238000011160 research Methods 0.000 description 3
- 238000005516 engineering process Methods 0.000 description 2
- 239000003205 fragrance Substances 0.000 description 2
- 230000000670 limiting effect Effects 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 238000005259 measurement Methods 0.000 description 2
- 230000008569 process Effects 0.000 description 2
- 230000001105 regulatory effect Effects 0.000 description 2
- 238000012360 testing method Methods 0.000 description 2
- ZWEHNKRNPOVVGH-UHFFFAOYSA-N 2-Butanone Chemical compound CCC(C)=O ZWEHNKRNPOVVGH-UHFFFAOYSA-N 0.000 description 1
- 238000003556 assay Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000008901 benefit Effects 0.000 description 1
- 238000004364 calculation method Methods 0.000 description 1
- 210000004081 cilia Anatomy 0.000 description 1
- 238000010276 construction Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 238000010790 dilution Methods 0.000 description 1
- 239000012895 dilution Substances 0.000 description 1
- 238000009472 formulation Methods 0.000 description 1
- 238000004817 gas chromatography Methods 0.000 description 1
- 230000036541 health Effects 0.000 description 1
- 230000007407 health benefit Effects 0.000 description 1
- 230000002427 irreversible effect Effects 0.000 description 1
- 238000004811 liquid chromatography Methods 0.000 description 1
- 230000007774 longterm Effects 0.000 description 1
- 230000014759 maintenance of location Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 231100000017 mucous membrane irritation Toxicity 0.000 description 1
- 230000008520 organization Effects 0.000 description 1
- 230000008447 perception Effects 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 238000003672 processing method Methods 0.000 description 1
- 238000000611 regression analysis Methods 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 238000002798 spectrophotometry method Methods 0.000 description 1
- 238000012421 spiking Methods 0.000 description 1
- 235000019505 tobacco product Nutrition 0.000 description 1
- 230000001988 toxicity Effects 0.000 description 1
- 231100000419 toxicity Toxicity 0.000 description 1
Images
Classifications
-
- 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
-
- 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
-
- 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
- G01N30/86—Signal analysis
- G01N30/8675—Evaluation, i.e. decoding of the signal into analytical information
- G01N30/8679—Target compound analysis, i.e. whereby a limited number of peaks is analysed
-
- 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
- G01N2030/042—Standards
- G01N2030/047—Standards external
-
- 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
Landscapes
- Physics & Mathematics (AREA)
- Health & Medical Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Chemical & Material Sciences (AREA)
- Analytical Chemistry (AREA)
- Biochemistry (AREA)
- General Health & Medical Sciences (AREA)
- General Physics & Mathematics (AREA)
- Immunology (AREA)
- Pathology (AREA)
- Engineering & Computer Science (AREA)
- Library & Information Science (AREA)
- Investigating Or Analyzing Non-Biological Materials By The Use Of Chemical Means (AREA)
Abstract
The invention relates to a method for simultaneously measuring the content of 8 carbonyl compounds in a cigarette bead, belonging to the technical field of physical and chemical inspection of cigarette materials. Extracting to-be-detected cigarette blasting beads by adopting acetonitrile through vortex oscillation, derivatizing supernatant obtained by extraction and a derivatizing reagent in the acetonitrile, filtering by using an organic phase filter membrane, and taking filtrate to obtain a sample solution; and finally, detecting and analyzing the sample solution and the blank solution by using a high performance liquid chromatograph, and quantifying by using an external standard method. The method has good separation effect on 8 objects to be measured, good peak shape, higher sensitivity, good repeatability and high recovery rate, and realizes the accurate determination of 8 carbonyl compounds in the cigarette blasting beads simultaneously, thereby improving the quality safety of cigarette products.
Description
Technical Field
The invention belongs to the technical field of physical and chemical inspection of cigarette materials, and particularly relates to a method capable of simultaneously detecting the content of 8 carbonyl compounds in a cigarette bead.
Background
The 'bead blasting addition' technology in the bead blasting filter stick is a cigarette filter tip production and forming technology, fragrance beads are implanted in the filter tip production process, controllable characteristic fragrance release in the cigarette smoking process is achieved, the influence of the external environment on the smoking taste and the loss of essence caused by the external environment are reduced, the cigarette smoking taste is enriched, and moisture retention and humidification in the smoking process are achieved. The puffed beads are a new technical way for perfuming, increasing aroma and keeping moisture of cigarettes, are effective supports for perception in the construction work of products, and are also means for realizing the youthfulness and individuation of cigarette brands.
Volatile carbonyl compounds have cilia toxicity and severe mucosal irritation, and can cause irreversible damage to the human body after long-term contact. Carbonyl compounds are also in the list of regulatory components proposed by the World Health Organization (WHO) "tobacco products regulatory research group". Currently, China mainly detects 8 carbonyl compounds contained in Hoffmann lists: formaldehyde, acetaldehyde, acetone, acrolein, propionaldehyde, crotonaldehyde, 2-butanone, and butyraldehyde. At present, a safety standard system of the cigarette bead blasting is gradually established, but the research on carbonyl compounds in the cigarette bead blasting is less. In order to further improve the safety of the cigarette bead blasting, ensure the quality safety of cigarette products, maintain the health benefits of consumers and ensure the continuous and healthy development of the industry, the establishment of a method for detecting 8 carbonyl compounds in the cigarette bead blasting is necessary.
At present, the current domestic and foreign research reports report that the common methods for detecting and analyzing the 8 carbonyl compounds comprise a spectrophotometry method, a gas chromatography method, a liquid chromatography method and the like. No report is found for simultaneously measuring 8 carbonyl compounds in the cigarette blasting beads.
Disclosure of Invention
The invention aims to provide a method for simultaneously measuring 8 carbonyl compounds in a cigarette bead so as to improve the safety of cigarette products, aiming at the defects of the prior art.
In order to achieve the purpose, the technical scheme adopted by the invention is as follows:
all percentages used herein are by weight unless otherwise indicated.
A method for simultaneously measuring 8 carbonyl compounds in cigarette blasting beads comprises the following steps:
step (1), preparation of a derivatization reagent: adding 2, 4-dinitrophenylhydrazine and phosphoric acid into acetonitrile, and uniformly mixing to obtain a derivatization reagent; the concentration of the 2, 4-dinitrophenylhydrazine in the derivatization reagent is 0.1 g/L; the volume percentage concentration of the phosphoric acid is 6 per mill;
step (2), preparation of sample solution and blank solution: putting the to-be-detected cigarette bead blasting into a centrifugal tube, adding acetonitrile and a homogeneous proton, carrying out vortex oscillation until all bead blasting samples are broken, and taking supernatant; the volume ratio of the mass of the cigarette blasting beads to the acetonitrile is 0.2 g: 10 mL;
adding the supernatant into the derivatization reagent prepared in the step (1), adding acetonitrile into the derivatization reagent, performing derivatization for 20min, filtering the mixture by using an organic phase filter membrane, and taking filtrate to obtain a sample solution; wherein the volume ratio of the supernatant, the derivatization reagent prepared in the step (1) and the reaction liquid after adding acetonitrile is 1: 4: 10;
the preparation method of the blank solution is the same except that no to-be-detected cigarette blasting beads are added into a centrifugal tube;
and (3) analyzing by high performance liquid chromatography: detecting and analyzing the sample solution and the blank solution by using a high performance liquid chromatograph; quantifying by an external standard method;
the high performance liquid chromatography adopts a gradient elution procedure, wherein a mobile phase A is acetonitrile; the mobile phase B is water; gradient elution procedure: 0 to 8min, 60% A; 8-9 min: the 60% a was linearly changed to 90% a; 9 to 14 min: 90% of A; 14 to 15 min: 90% A was linearly changed to 60% A; 15-20 min: 60% of A.
Further, it is preferable that the HPLC analysis is performed under the condition of using AcclaimTMExposives E2C 185 μm 4.6X 250mm column; column temperature: 30 ℃; column flow rate: 1.0 mL/min; sample introduction amount: 10 mu L of the solution; and a diode array detector is adopted, and the detection wavelength is 365 nm.
Further, preferably, the specific method for quantifying by the external standard method is as follows:
s1, preparing a mixed standard stock solution: weighing 10mg of 2, 4-dinitrophenylhydrazone derivative compounds of formaldehyde, acetaldehyde, acetone, acrolein, propionaldehyde, crotonaldehyde, 2-butyraldehyde and butyraldehyde respectively, placing the compounds in a 100mL volumetric flask, dissolving the compounds with acetonitrile, and fixing the volume to a scale to obtain a mixed standard stock solution;
s2, mixing standard solutions: accurately transferring 10mL of mixed standard stock solution into a 100mL volumetric flask, and carrying out constant volume by using acetonitrile to prepare the mixed standard solution.
S3, preparing a standard working solution: accurately transferring 100 mu L, 200 mu L, 500 mu L, 1000 mu L, 2000 mu L and 4000 mu L of mixed standard solution into a 10mL volumetric flask, and fixing the volume to the scale by acetonitrile;
s4, establishing a standard working curve: converting 2, 4-dinitrophenylhydrazone derivative compounds of formaldehyde, acetaldehyde, acetone, acrolein, propionaldehyde, crotonaldehyde, 2-butyraldehyde and butyraldehyde into the concentrations of the formaldehyde, the acetaldehyde, the acetone, the acrolein, the propionaldehyde, the crotonaldehyde, 2-butyraldehyde and the butyraldehyde, establishing a working curve of the standard working solution by using the peak areas of hydrazone in the standard working solution corresponding to the equivalent concentrations of the formaldehyde, the acetaldehyde, the acetone, the acrolein, the propionaldehyde, the crotonaldehyde, the 2-butyraldehyde and the butyraldehyde, wherein the conversion formula is as follows:
Cformaldehyde (I)=0.1422CFormaldehyde-2, 4-dinitrophenylhydrazone（1）
CAcetaldehyde=0.1957CAcetaldehyde-2, 4-dinitrophenylhydrazone（2）
CAcetone (II)=0.2428CAcetone-2, 4-dinitrophenylhydrazone（3）
CAcrolein=0.2364CAcrolein-2, 4-dinitrophenylhydrazone（4）
CPropionaldehyde=0.2428CPropanal-2, 4-dinitrophenylhydrazone（5）
CCrotonaldehyde=0.2790CCrotonaldehyde-2, 4-dinitrophenylhydrazone（6）
C2-butyraldehyde=0.2848C2-butyraldehyde-2, 4-dinitrophenylhydrazone（7）
CButyraldehyde=0.2848CButyraldehyde-2, 4-dinitrophenylhydrazone（8）
S5, calculating a result: and substituting the chromatographic peak areas of the 2, 4-dinitrophenylhydrazone derivative compounds of the blank solution and the sample solution, which are measured under the same condition, into the standard working curve obtained by S4 to obtain the concentrations of formaldehyde, acetaldehyde, acetone, acrolein, propionaldehyde, crotonaldehyde, 2-butyraldehyde and butyraldehyde, so as to obtain the contents of the formaldehyde, the acetaldehyde, the acetone, the acrolein, the propionaldehyde, the crotonaldehyde, the 2-butyraldehyde and the butyraldehyde in the blasting bead of the cigarette to be measured.
Further, preferably, the method for simultaneously determining 8 carbonyl compounds in the cigarette blasting beads comprises the following steps:
step (1), preparation of a derivatization reagent: weighing 0.1g of 2, 4-dinitrophenylhydrazine in a 1000mL brown bottle, adding 6mL of phosphoric acid, and diluting to the constant volume with acetonitrile;
step (2), preparation of sample solution: weighing 0.2g of cigarette blasting beads to be detected, adding 10mL of acetonitrile and a ceramic homogeneous proton into a 50mL centrifuge tube, performing vortex oscillation in a pulse mode for 10min, and standing for 2 min; accurately transferring 1.0mL of supernatant into a 10mL volumetric flask, adding 4mL of derivatization reagent, then diluting to the constant volume with acetonitrile, shaking up, standing at room temperature for 30min for derivatization, filtering through a 0.45-micrometer organic phase filter membrane, and then taking filtrate to obtain a sample solution;
the preparation method of the blank solution is the same except that no to-be-detected cigarette blasting beads are added into a centrifugal tube;
and (3) analyzing by high performance liquid chromatography: detecting and analyzing the sample solution and the blank solution by using a high performance liquid chromatograph; quantification by external standard method.
Compared with the prior art, the invention has the beneficial effects that:
(1) the invention provides a method for measuring 8 carbonyl compounds in a cigarette blasting bead, which realizes the accurate measurement of the 8 carbonyl compounds in the cigarette blasting bead simultaneously, thereby improving the quality safety of cigarette products.
(2) The invention improves and optimizes the sample processing method and the chromatographic condition, adopts the vortex oscillation to break the wall and then uses the acetonitrile solution to extract, and has good separation effect and peak shape of 8 objects to be detected.
(3) The chromatographic conditions adopted by the method of the invention ensure that the chromatographic peak separation degrees of 8 compounds to be detected are all good, and the compounds have good linear correlation, the detection limit is 1.13mg/kg of formaldehyde, 1.26mg/kg of acetaldehyde, 1.51mg/kg of acetone, 1.76mg/kg of acrolein, 1.00mg/kg of propionaldehyde, 1.14mg/kg of crotonaldehyde, 1.33mg/kg of 2-butyraldehyde and 1.98mg/kg of butyraldehyde, and the sensitivity of the method is high.
(4) The recovery rate of formaldehyde is 98.64%, the recovery rate of acetaldehyde is 97.85%, acetone 97.39%, acrolein 96.51%, propionaldehyde 95.31%, crotonaldehyde 98.70%, 2-butyraldehyde 98.32% and butyraldehyde 96.46% are all less than 5.0%, and the method has high recovery rate and good repeatability.
Drawings
FIG. 1 is a flow chart of the assay method of the present invention;
FIG. 2 is a chromatogram of a standard working solution; wherein, 1-formaldehyde-DNPH; 2-acetaldehyde-DNPH; 3-acetone-DNPH; 4-acrolein-DNPH; 5-propanal-DNPH; 6-crotonaldehyde-DNPH; 7-2-butyraldehyde-DNPH; 8-butyraldehyde-DNPH;
FIG. 3 is a diagram of chromatographic analysis of a sample solution; wherein, 1-formaldehyde-DNPH; 2-acetone-DNPH
FIG. 4 is a standard curve of formaldehyde;
FIG. 5 is a graph of acetaldehyde standard curve;
FIG. 6 is a graph of acetone standard curves;
FIG. 7 is a standard curve diagram of acrolein;
FIG. 8 is a propionaldehyde standard curve;
FIG. 9 is a standard graph of crotonaldehyde;
FIG. 10 is a graph of the standard 2-butyraldehyde plot;
FIG. 11 is a butyraldehyde standard curve.
Detailed Description
The present invention will be described in further detail with reference to examples.
It will be appreciated by those skilled in the art that the following examples are illustrative of the invention only and should not be taken as limiting the scope of the invention. The examples do not specify particular techniques or conditions, and are performed according to the techniques or conditions described in the literature in the art or according to the product specifications. The materials or equipment used are not indicated by manufacturers, and all are conventional products available by purchase.
Example 1
A method for simultaneously measuring 8 carbonyl compounds in cigarette blasting beads comprises the following steps:
step (1), preparation of a derivatization reagent: adding 2, 4-dinitrophenylhydrazine and phosphoric acid into acetonitrile, and uniformly mixing to obtain a derivatization reagent; the concentration of the 2, 4-dinitrophenylhydrazine in the derivatization reagent is 0.1 g/L; the volume percentage concentration of the phosphoric acid is 6 per mill;
step (2), preparation of sample solution and blank solution: putting the to-be-detected cigarette bead blasting into a centrifugal tube, adding acetonitrile and a homogeneous proton, carrying out vortex oscillation until all bead blasting samples are broken, and taking supernatant; the volume ratio of the mass of the cigarette blasting beads to the acetonitrile is 0.2 g: 10 mL;
adding the supernatant into the derivatization reagent prepared in the step (1), adding acetonitrile into the derivatization reagent, performing derivatization for 20min, filtering the mixture by using an organic phase filter membrane, and taking filtrate to obtain a sample solution; wherein the volume ratio of the supernatant, the derivatization reagent prepared in the step (1) and the reaction liquid after adding acetonitrile is 1: 4: 10;
the preparation method of the blank solution is the same except that no to-be-detected cigarette blasting beads are added into a centrifugal tube;
and (3) analyzing by high performance liquid chromatography: detecting and analyzing the sample solution and the blank solution by using a high performance liquid chromatograph; quantifying by an external standard method;
the high performance liquid chromatography adopts a gradient elution procedure, wherein a mobile phase A is acetonitrile; the mobile phase B is water; gradient elution procedure: 0 to 8min, 60% A; 8-9 min: the 60% a was linearly changed to 90% a; 9 to 14 min: 90% of A; 14 to 15 min: 90% A was linearly changed to 60% A; 15-20 min: 60% of A.
Example 2
A method for simultaneously measuring 8 carbonyl compounds in cigarette blasting beads comprises the following steps:
step (1), preparation of a derivatization reagent: weighing 0.1g of 2, 4-dinitrophenylhydrazine in a 1000mL brown bottle, adding 6mL of phosphoric acid, and diluting to the constant volume with acetonitrile;
step (2), preparation of sample solution: weighing 0.2g of cigarette blasting beads to be detected, adding 10mL of acetonitrile and a ceramic homogeneous proton into a 50mL centrifuge tube, performing vortex oscillation in a pulse mode for 10min, and standing for 2 min; accurately transferring 1.0mL of supernatant into a 10mL volumetric flask, adding 4mL of derivatization reagent, then diluting to the constant volume with acetonitrile, shaking up, standing at room temperature for 30min for derivatization, filtering through a 0.45-micrometer organic phase filter membrane, and then taking filtrate to obtain a sample solution;
the preparation method of the blank solution is the same except that no to-be-detected cigarette blasting beads are added into a centrifugal tube;
and (3) analyzing by high performance liquid chromatography: detecting and analyzing the sample solution and the blank solution by using a high performance liquid chromatograph; quantification by external standard method.
The high performance liquid chromatography adopts a gradient elution procedure, wherein a mobile phase A is acetonitrile; the mobile phase B is water; gradient elution procedure: 0 to 8min, 60% A; 8-9 min: the 60% a was linearly changed to 90% a; 9 to 14 min: 90% of A; 14 to 15 min: 90% A was linearly changed to 60% A; 15-20 min: 60% of A.
The high performance liquid chromatography analysis adopts Acclaim as chromatographic conditionTMExposives E2C 185 μm 4.6X 250mm column; column temperature: 30 ℃; column flow rate: 1.0 mL/min; sample introduction amount: 10 mu L of the solution; and a diode array detector is adopted, and the detection wavelength is 365 nm.
The specific method for quantifying by the external standard method comprises the following steps:
s1, preparing a mixed standard stock solution: weighing 10mg of 2, 4-dinitrophenylhydrazone derivative compounds of formaldehyde, acetaldehyde, acetone, acrolein, propionaldehyde, crotonaldehyde, 2-butyraldehyde and butyraldehyde respectively, placing the compounds in a 100mL volumetric flask, dissolving the compounds with acetonitrile, and fixing the volume to a scale to obtain a mixed standard stock solution;
s2, mixing standard solutions: accurately transferring 10mL of mixed standard stock solution into a 100mL volumetric flask, and carrying out constant volume by using acetonitrile to prepare the mixed standard solution.
S3, preparing a standard working solution: accurately transferring 100 mu L, 200 mu L, 500 mu L, 1000 mu L, 2000 mu L and 4000 mu L of mixed standard solution into a 10mL volumetric flask, and fixing the volume to the scale by acetonitrile;
s4, establishing a standard working curve: converting 2, 4-dinitrophenylhydrazone derivative compounds of formaldehyde, acetaldehyde, acetone, acrolein, propionaldehyde, crotonaldehyde, 2-butyraldehyde and butyraldehyde into the concentrations of the formaldehyde, the acetaldehyde, the acetone, the acrolein, the propionaldehyde, the crotonaldehyde, 2-butyraldehyde and the butyraldehyde, establishing a working curve of the standard working solution by using the peak areas of hydrazone in the standard working solution corresponding to the equivalent concentrations of the formaldehyde, the acetaldehyde, the acetone, the acrolein, the propionaldehyde, the crotonaldehyde, the 2-butyraldehyde and the butyraldehyde, wherein the conversion formula is as follows:
Cformaldehyde (I)=0.1422CFormaldehyde-2, 4-dinitrophenylhydrazone（1）
CAcetaldehyde=0.1957CAcetaldehyde-2, 4-dinitrophenylhydrazone（2）
CAcetone (II)=0.2428CAcetone-2, 4-dinitrophenylhydrazone（3）
CAcrolein=0.2364CAcrolein-2, 4-dinitrophenylhydrazone（4）
CPropionaldehyde=0.2428CPropanal-2, 4-bisNitrobenzenehydrazones（5）
CCrotonaldehyde=0.2790CCrotonaldehyde-2, 4-dinitrophenylhydrazone（6）
C2-butyraldehyde=0.2848C2-butyraldehyde-2, 4-dinitrophenylhydrazone（7）
CButyraldehyde=0.2848CButyraldehyde-2, 4-dinitrophenylhydrazone（8）
S5, calculating a result: and substituting the chromatographic peak areas of the 2, 4-dinitrophenylhydrazone derivative compounds of the blank solution and the sample solution, which are measured under the same condition, into the standard working curve obtained by S4 to obtain the concentrations of formaldehyde, acetaldehyde, acetone, acrolein, propionaldehyde, crotonaldehyde, 2-butyraldehyde and butyraldehyde, so as to obtain the contents of the formaldehyde, the acetaldehyde, the acetone, the acrolein, the propionaldehyde, the crotonaldehyde, the 2-butyraldehyde and the butyraldehyde in the blasting bead of the cigarette to be measured.
Example 3
A method for simultaneously measuring 8 carbonyl compounds in cigarette blasting beads comprises the following steps:
(1) preparation of mixed standard stock solution: weighing 10mg of 2, 4-dinitrophenylhydrazone derivative compounds of formaldehyde, acetaldehyde, acetone, acrolein, propionaldehyde, crotonaldehyde, 2-butyraldehyde and butyraldehyde respectively, placing the compounds in a 100mL volumetric flask, dissolving the compounds with acetonitrile, and fixing the volume to a scale to obtain a mixed standard stock solution.
(2) Mixing standard solutions: accurately transferring 10mL of mixed standard stock solution into a 100mL volumetric flask, and carrying out constant volume by using acetonitrile to prepare the mixed standard solution.
(3) Preparation of standard working solution: and preparing a series of standard working solutions with proper concentration according to the actual content of the sample. The series of standard working solutions are prepared by taking acetonitrile as a solvent and diluting the mixed standard solutions. The following formulation method is recommended: accurately transferring 100 mu L, 200 mu L, 500 mu L, 1000 mu L, 2000 mu L and 4000 mu L of mixed standard solution into a 10mL volumetric flask, and fixing the volume to the scale with acetonitrile.
(4) Establishing a standard working curve: detecting and analyzing the standard working solutions with 6 concentration levels by using a high performance liquid chromatograph; converting 2, 4-dinitrophenylhydrazone derivative compounds of formaldehyde, acetaldehyde, acetone, acrolein, propionaldehyde, crotonaldehyde, 2-butyraldehyde and butyraldehyde into the concentrations of the formaldehyde, the acetaldehyde, the acetone, the acrolein, the propionaldehyde, the crotonaldehyde, 2-butyraldehyde and the butyraldehyde, establishing a working curve of the standard working solution by using the peak areas of hydrazone in the standard working solution corresponding to the equivalent concentrations of the formaldehyde, the acetaldehyde, the acetone, the acrolein, the propionaldehyde, the crotonaldehyde, the 2-butyraldehyde and the butyraldehyde, wherein the conversion formula is as follows:
Cformaldehyde (I)=0.1422CFormaldehyde-2, 4-dinitrophenylhydrazone（1）
CAcetaldehyde=0.1957CAcetaldehyde-2, 4-dinitrophenylhydrazone（2）
CAcetone (II)=0.2428CAcetone-2, 4-dinitrophenylhydrazone（3）
CAcrolein=0.2364CAcrolein-2, 4-dinitrophenylhydrazone（4）
CPropionaldehyde=0.2428CPropanal-2, 4-dinitrophenylhydrazone（5）
CCrotonaldehyde=0.2790CCrotonaldehyde-2, 4-dinitrophenylhydrazone（6）
C2-butyraldehyde=0.2848C2-butyraldehyde-2, 4-dinitrophenylhydrazone（7）
CButyraldehyde=0.2848CButyraldehyde-2, 4-dinitrophenylhydrazone（8）
(5) Preparation of derivatization reagent: weighing 0.1g of 2, 4-dinitrophenylhydrazine in a 1000mL brown bottle, adding 6mL of phosphoric acid, and diluting to the constant volume with acetonitrile;
(6) preparation of sample solution: weighing 0.2g of cigarette blasting beads to be detected, adding 10mL of acetonitrile and a ceramic homogeneous proton into a 50mL centrifuge tube, performing vortex oscillation in a pulse mode for 10min, and standing for 2 min; accurately transferring 1.0mL of supernatant into a 10mL volumetric flask, adding 4mL of derivatization reagent, diluting to a constant volume with acetonitrile, shaking uniformly, standing at room temperature for 30min for derivatization, filtering with a 0.45-micrometer organic phase filter membrane, and taking filtrate to obtain a sample solution;
the preparation method of the blank solution is the same except that no to-be-detected cigarette blasting beads are added into a centrifugal tube;
(7) high performance liquid chromatography analysis: respectively detecting and analyzing the sample solution and the blank solution by using a high performance liquid chromatograph;
(8) and (4) calculating a result: and (3) substituting the chromatographic peak areas of the 2, 4-dinitrophenylhydrazone derivative compounds of the formaldehyde, the acetaldehyde, the acetone, the acrolein, the propionaldehyde, the crotonaldehyde, the 2-butyraldehyde and the butyraldehyde in the sample solution and the blank solution under the same condition into the standard working curve obtained in the step (4) to obtain the concentrations of the formaldehyde, the acetaldehyde, the acetone, the crotonaldehyde, the 2-butyraldehyde and the butyraldehyde, so as to obtain the contents of the formaldehyde, the acetaldehyde, the acetone, the acrolein, the propionaldehyde, the crotonaldehyde, the 2-butyraldehyde and the butyraldehyde in the blasting bead of the cigarette to be detected.
The high performance liquid chromatography analysis adopts Acclaim as chromatographic conditionTMExposives E2C 185 μm 4.6X 250mm column; column temperature: 30 ℃; mobile phase A: acetonitrile; mobile phase B: water; gradient elution procedure: 0 to 8min, 60% A; 8-9 min: the 60% a was linearly changed to 90% a; 9 to 14 min: 90% of A; 14 to 15 min: 90% A was linearly changed to 60% A; 15-20 min: 60% of A; column flow rate: 1.0 mL/min; sample introduction amount: 10 mu L of the solution; and a diode array detector is adopted, and the detection wavelength is 365 nm.
Application example 1
Measuring the content of 8 carbonyl compounds in the cigarette blasting beads (the flow of the measuring method is shown in figure 1);
1. preparation of Standard working solutions
(1) Preparation of mixed standard stock solution: weighing 10mg of 2, 4-dinitrophenylhydrazone derivative compounds of formaldehyde, acetaldehyde, acetone, acrolein, propionaldehyde, crotonaldehyde, 2-butyraldehyde and butyraldehyde respectively, placing the compounds in a 100mL volumetric flask, dissolving the compounds with acetonitrile, and fixing the volume to a scale to obtain a mixed standard stock solution;
(2) preparation of standard working solution: transferring 0.5mL of mixed standard stock solution into a 50mL volumetric flask, dissolving and uniformly mixing with acetonitrile, and fixing the volume to a scale to obtain a 1 st-level standard working solution; adding 20.00mL of the 1 st-level standard working solution into a 50mL volumetric flask, dissolving and uniformly mixing with acetonitrile, and fixing the volume to a scale to obtain a 2 nd-level standard working solution; adding 20.00mL of the 2 nd-level standard working solution into a 50mL volumetric flask, dissolving and uniformly mixing with acetonitrile, and fixing the volume to a scale to obtain a 3 rd-level standard working solution; adding 20.00mL of the 3 rd-level standard working solution into a 50mL volumetric flask, dissolving and uniformly mixing with acetonitrile, and fixing the volume to a scale to obtain a 4 th-level standard working solution; adding 20.00mL of the 4 th-level standard working solution into a 50mL volumetric flask, dissolving and uniformly mixing with acetonitrile, and fixing the volume to a scale to obtain a 5 th-level standard working solution; adding 20.00mL of the 5 th-level standard working solution into a 50mL volumetric flask, dissolving and uniformly mixing with acetonitrile, and fixing the volume to a scale to obtain a 6 th-level standard working solution;
2. preparation of sample solution and blank solution
(1) Preparation of a sample solution: accurately weighing 0.2g (accurate to 0.1 mg) of a sample, adding 10mL of acetonitrile (used as an extract) and a ceramic homogeneous proton into a 50mL centrifuge tube, carrying out vortex oscillation for 10min in a pulse form, standing for 2min, accurately transferring 1.0mL of supernatant into a 10mL volumetric flask, adding 4mL of derivatization reagent, carrying out constant volume with acetonitrile, shaking uniformly, standing for 30min at room temperature for derivatization, and filtering through a 0.45-micrometer organic phase filter membrane to obtain a filtrate, namely a sample solution.
(2) Preparing a blank solution: the sample is not added into the centrifuge tube, and the same product solution is prepared in other processing steps;
3. chromatography analysis
Respectively taking the standard working solution, the blank solution and the sample solution for chromatographic analysis, wherein the chromatographic conditions adopt an Acclaim Exposives E2C 185 mu m4.6 multiplied by 250mm column; column temperature: 30 ℃; mobile phase A: acetonitrile; mobile phase B: water; gradient elution procedure: 0 to 8min, 60% A; 8-9 min: the 60% a was linearly changed to 90% a; 9 to 14 min: 90% of A; 14 to 15 min: 90% A was linearly changed to 60% A; 15-20 min: 60% of A; column flow rate: 1.0 mL/min; sample introduction amount: 10 mu L of the solution; and a diode array detector is adopted, and the detection wavelength is 365 nm. The results of the chromatographic analysis of the standard working solution and the sample solution are shown in FIGS. 2 and 3, respectively.
4. Drawing standard curve and calculating result
Firstly, performing regression analysis on concentrations of 2, 4-dinitrophenylhydrazone derivative compounds of formaldehyde, acetaldehyde, acetone, acrolein, propionaldehyde, crotonaldehyde, 2-butyraldehyde and butyraldehyde by using chromatographic peak areas of the 2, 4-dinitrophenylhydrazone derivative compounds of the formaldehyde, the acetaldehyde, the acetone, the acrolein, the propionaldehyde, the crotonaldehyde, the 2-butyraldehyde and the butyraldehyde to obtain standard curves, wherein the standard working curve results of the formaldehyde, the acetaldehyde, the acetone, the acrolein, the propionaldehyde, the crotonaldehyde, the 2-butyraldehyde and the butyraldehyde are respectively shown in a figure 4, a figure 5, a figure 6, a figure 7, a figure 8, a figure 9, a figure 10 and a figure 11, a minimum concentration working standard solution is taken to perform six times of parallel tests, the standard deviation is calculated, the 3-fold standard deviation is a detection limit, the 10-fold standard deviation is a quantitative detection limit;
TABLE 1 Standard Curve, detection Limit and quantification Limit of the carbonyl Compounds in the bead blasting of cigarettes
And then substituting the measured chromatographic peak areas of the two target compounds into the drawn standard curve to obtain the concentrations of the two target compounds in the sample, wherein the calculation formula is as follows:
x-the content of each carbonyl compound in the cigarette bead to be detected, wherein the unit is milligram per kilogram (mg/kg);
c-concentration of 8 carbonyl compounds in milligrams per liter (mg/L) from a standard curve;
C0-blank values from the standard curve in milligrams per liter (mg/L);
v-volume of extract in milliliters (mL);
m is the mass of the cigarette bead to be detected, and the unit is gram (g);
je-dilution factor of the sample solution.
TABLE 2 detection results of the contents of 8 kinds of carbonyl compounds in the blasting beads of cigarettes produced in a certain country
As can be seen from Table 1, the chromatographic conditions employed gave a good degree of separation of all 8 target compounds and a good linear correlation, with a detection limit for formaldehyde of 0.70mg/kg, for acetaldehyde of 0.78mg/kg, for acetone of 0.93mg/kg, for acrolein of 1.09mg/kg, for propionaldehyde of 0.62mg/kg, for crotonaldehyde of 0.70mg/kg, for 2-butyraldehyde of 0.93mg/kg and for butyraldehyde of 1.63 mg/kg.
Application example 2
This example tests the reproducibility and spiking recovery of the method of the invention.
1. Preparation of standard working solutions: the same as in example 1.
2. Adding 3 gradient standard solutions into samples respectively, wherein formaldehyde and acetone are added at three levels of 10, 20 and 40mg/kg, other 6 carbonyl compounds are added at three levels of 5, 10 and 20mg/kg, the chromatographic analysis conditions are the same as the chromatographic analysis conditions of example 1, each sample is measured for 6 times respectively, and the standard average recovery rate of the cigarette popping beads and the relative standard deviation of the measured value after the calibration are calculated according to the analysis results, and the results are shown in table 3.
TABLE 3 results of recovery with standard addition and standard deviation
As can be seen from Table 3, the average relative standard deviation of formaldehyde is 2.45%, the average relative standard deviation of acetaldehyde is 3.04%, the average recovery rate of formaldehyde is 98.14%, and the recovery rate of acetaldehyde is 97.55%, indicating that the method has good precision and high recovery rate.
The standard solution used in this example is only illustrated by taking one concentration value as an example, and the standard curve and regression equation obtained by chromatographic analysis of other prepared standard solutions are the same as those in the above example, and only the positions of the scatter diagram and the scatter point are different, and the measurement result of the sample is not affected, and are not listed here. The embodiments are only used for better understanding of the present invention, and do not have any limiting effect, that is, the above methods or places used in the above situations are all included in the technical scope of the present invention.
The foregoing shows and describes the general principles, essential features, and advantages of the invention. It will be understood by those skilled in the art that the present invention is not limited to the embodiments described above, which are described in the specification and illustrated only to illustrate the principle of the present invention, but that various changes and modifications may be made therein without departing from the spirit and scope of the present invention, which fall within the scope of the invention as claimed. The scope of the invention is defined by the appended claims and equivalents thereof.
Claims (4)
1. A method for simultaneously measuring 8 carbonyl compounds in cigarette blasting beads is characterized by comprising the following steps:
step (1), preparation of a derivatization reagent: adding 2, 4-dinitrophenylhydrazine and phosphoric acid into acetonitrile, and uniformly mixing to obtain a derivatization reagent; the concentration of the 2, 4-dinitrophenylhydrazine in the derivatization reagent is 0.1 g/L; the volume percentage concentration of the phosphoric acid is 6 per mill;
step (2), preparation of sample solution and blank solution: putting the to-be-detected cigarette bead blasting into a centrifugal tube, adding acetonitrile and a homogeneous proton, carrying out vortex oscillation until all bead blasting samples are broken, and taking supernatant; the volume ratio of the mass of the cigarette blasting beads to the acetonitrile is 0.2 g: 10 mL;
adding the supernatant into the derivatization reagent prepared in the step (1), adding acetonitrile into the derivatization reagent, performing derivatization for 20min, filtering the mixture by using an organic phase filter membrane, and taking filtrate to obtain a sample solution; wherein the volume ratio of the supernatant, the derivatization reagent prepared in the step (1) and the reaction liquid after adding acetonitrile is 1: 4: 10;
the preparation method of the blank solution is the same except that no to-be-detected cigarette blasting beads are added into a centrifugal tube;
and (3) analyzing by high performance liquid chromatography: detecting and analyzing the sample solution and the blank solution by using a high performance liquid chromatograph; quantifying by an external standard method;
the high performance liquid chromatography adopts a gradient elution procedure, wherein a mobile phase A is acetonitrile; the mobile phase B is water; gradient elution procedure: 0 to 8min, 60% A; 8-9 min: the 60% a was linearly changed to 90% a; 9 to 14 min: 90% of A; 14 to 15 min: 90% A was linearly changed to 60% A; 15-20 min: 60% of A.
2. The method for simultaneously determining 8 carbonyl compounds in cigarette blasting beads according to claim 1, wherein the HPLC analysis is performed under the condition of AcclaimTMExposives E2C 185 μm 4.6X 250mm column; column temperature: 30 ℃; column flow rate: 1.0 mL/min; sample introduction amount: 10 mu L of the solution; and a diode array detector is adopted, and the detection wavelength is 365 nm.
3. The method for simultaneously determining 8 carbonyl compounds in the cigarette blasting bead according to claim 1, characterized in that the specific method for external standard method quantification is as follows:
s1, preparing a mixed standard stock solution: weighing 10mg of 2, 4-dinitrophenylhydrazone derivative compounds of formaldehyde, acetaldehyde, acetone, acrolein, propionaldehyde, crotonaldehyde, 2-butyraldehyde and butyraldehyde respectively, placing the compounds in a 100mL volumetric flask, dissolving the compounds with acetonitrile, and fixing the volume to a scale to obtain a mixed standard stock solution;
s2, mixing standard solutions: accurately transferring 10mL of mixed standard stock solution into a 100mL volumetric flask, and carrying out constant volume by using acetonitrile to prepare the mixed standard solution.
S3, preparing a standard working solution: accurately transferring 100 mu L, 200 mu L, 500 mu L, 1000 mu L, 2000 mu L and 4000 mu L of mixed standard solution into a 10mL volumetric flask, and fixing the volume to the scale by acetonitrile;
s4, establishing a standard working curve: converting 2, 4-dinitrophenylhydrazone derivative compounds of formaldehyde, acetaldehyde, acetone, acrolein, propionaldehyde, crotonaldehyde, 2-butyraldehyde and butyraldehyde into the concentrations of the formaldehyde, the acetaldehyde, the acetone, the acrolein, the propionaldehyde, the crotonaldehyde, 2-butyraldehyde and the butyraldehyde, establishing a working curve of the standard working solution by using the peak areas of hydrazone in the standard working solution corresponding to the equivalent concentrations of the formaldehyde, the acetaldehyde, the acetone, the acrolein, the propionaldehyde, the crotonaldehyde, the 2-butyraldehyde and the butyraldehyde, wherein the conversion formula is as follows:
Cformaldehyde (I)=0.1422CFormaldehyde-2, 4-dinitrophenylhydrazone（1）
CAcetaldehyde=0.1957CAcetaldehyde-2, 4-dinitrophenylhydrazone（2）
CAcetone (II)=0.2428CAcetone-2, 4-dinitrophenylhydrazone（3）
CAcrolein=0.2364CAcrolein-2, 4-dinitrophenylhydrazone（4）
CPropionaldehyde=0.2428CPropanal-2, 4-dinitrophenylhydrazone（5）
CCrotonaldehyde=0.2790CCrotonaldehyde-2, 4-dinitrophenylhydrazone（6）
C2-butyraldehyde=0.2848C2-butyraldehyde-2, 4-dinitrophenylhydrazone（7）
CButyraldehyde=0.2848CButyraldehyde-2, 4-dinitrophenylhydrazone（8）
S5, calculating a result: and substituting the chromatographic peak areas of the 2, 4-dinitrophenylhydrazone derivative compounds of the blank solution and the sample solution, which are measured under the same condition, into the standard working curve obtained by S4 to obtain the concentrations of formaldehyde, acetaldehyde, acetone, acrolein, propionaldehyde, crotonaldehyde, 2-butyraldehyde and butyraldehyde, so as to obtain the contents of the formaldehyde, the acetaldehyde, the acetone, the acrolein, the propionaldehyde, the crotonaldehyde, the 2-butyraldehyde and the butyraldehyde in the blasting bead of the cigarette to be measured.
4. The method for simultaneously determining 8 carbonyl compounds in a cigarette bead according to claim 1, comprising the steps of:
step (1), preparation of a derivatization reagent: weighing 0.1g of 2, 4-dinitrophenylhydrazine in a 1000mL brown bottle, adding 6mL of phosphoric acid, and diluting to the constant volume with acetonitrile;
step (2), preparation of sample solution: weighing 0.2g of cigarette blasting beads to be detected, adding 10mL of acetonitrile and a ceramic homogeneous proton into a 50mL centrifuge tube, performing vortex oscillation in a pulse mode for 10min, and standing for 2 min; accurately transferring 1.0mL of supernatant into a 10mL volumetric flask, adding 4mL of derivatization reagent, then diluting to the constant volume with acetonitrile, shaking up, standing at room temperature for 30min for derivatization, filtering through a 0.45-micrometer organic phase filter membrane, and then taking filtrate to obtain a sample solution;
the preparation method of the blank solution is the same except that no to-be-detected cigarette blasting beads are added into a centrifugal tube;
and (3) analyzing by high performance liquid chromatography: detecting and analyzing the sample solution and the blank solution by using a high performance liquid chromatograph; quantification by external standard method.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202010048812.9A CN111208227A (en) | 2020-01-16 | 2020-01-16 | Method for simultaneously determining content of 8 carbonyl compounds in cigarette blasting beads |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202010048812.9A CN111208227A (en) | 2020-01-16 | 2020-01-16 | Method for simultaneously determining content of 8 carbonyl compounds in cigarette blasting beads |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN111208227A true CN111208227A (en) | 2020-05-29 |
Family
ID=70783487
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202010048812.9A Pending CN111208227A (en) | 2020-01-16 | 2020-01-16 | Method for simultaneously determining content of 8 carbonyl compounds in cigarette blasting beads |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN111208227A (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112748210A (en) * | 2020-12-29 | 2021-05-04 | 南京美思德新材料有限公司 | Method for determining aldehyde ketone content in polyether modified organic silicon |
-
2020
- 2020-01-16 CN CN202010048812.9A patent/CN111208227A/en active Pending
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112748210A (en) * | 2020-12-29 | 2021-05-04 | 南京美思德新材料有限公司 | Method for determining aldehyde ketone content in polyether modified organic silicon |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN104614466B (en) | The assay method of antiseptic in tobacco juice for electronic smoke | |
| Roach et al. | Capillary gas chromatography/mass spectrometry with chemical ionization and negative ion detection for confirmation of identity of patulin in apple juice | |
| CN116429943A (en) | Quality analysis method of traditional Chinese medicine radix scutellariae based on dual-wavelength equal-baseline differential fusion map | |
| CN116148387A (en) | Catecholamine and catecholamine metabolite detection method and kit | |
| Thuan et al. | Elimination of caffeine interference in HPLC determination of urinary nicotine and cotinine. | |
| CN107966518B (en) | Treatment method of smokeless tobacco product and determination method of small molecular aldehyde in smokeless tobacco product | |
| CN111208227A (en) | Method for simultaneously determining content of 8 carbonyl compounds in cigarette blasting beads | |
| AU2020102127A4 (en) | Collection and determination of acrolein and other four aldehydes in workplace | |
| CN111855866A (en) | Method for rapidly determining formaldehyde in tobacco additive | |
| CN108732272B (en) | HPLC detection method for benzyl chloride residue in enoxaparin sodium | |
| CN113219089B (en) | Method for detecting urea by post-column derivatization-liquid chromatography | |
| CN114280206A (en) | Method for detecting mycotoxin in spice and product thereof | |
| CN107831228B (en) | Method and kit for determining citronellal in sample and application of kit | |
| CN104897821A (en) | Method and kit for extracting inositol in sample, and application of kit | |
| CN111707754A (en) | Method for measuring guaiacol, ortho-vanillin, 5-methyl vanillin and 5-aldehyde vanillin in vanillin | |
| CN111751466A (en) | Method for simultaneously determining DON toxin and NIV toxin | |
| CN103983731B (en) | A kind of method measuring ortho-aminobenzoic acid cinnamic ester in essence and flavoring agent | |
| CN112198249B (en) | Detection method of ethanolamine compound in soil | |
| CN114814009B (en) | Analysis method simultaneously applicable to phenolic compounds in novel tobacco products and metabolites of phenolic compounds in urine | |
| CN113777197B (en) | Method for simultaneously determining citrinin and 1-hydroxy-2-naphthoic acid | |
| CN113533576B (en) | Method for detecting polyphenol compounds in cigars | |
| CN113640415B (en) | Method for detecting content of alpha-androstanol in truffle sporocarp | |
| CN113720934B (en) | Method for detecting aroma components in main stream smoke of cigarettes | |
| CN112710773B (en) | Method for simultaneously detecting fosfomycin and diol thereof by adopting ion chromatography | |
| CN112903856B (en) | Pretreatment method for detecting trace chloroformyl compound in water sample and application thereof |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| RJ01 | Rejection of invention patent application after publication | ||
| RJ01 | Rejection of invention patent application after publication |
Application publication date: 20200529 |