WO2023065811A1 - Procédé de mesure de teneur en méthanol dans une huile essentielle de bille à éclater de cigarette - Google Patents
Procédé de mesure de teneur en méthanol dans une huile essentielle de bille à éclater de cigarette Download PDFInfo
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- WO2023065811A1 WO2023065811A1 PCT/CN2022/114449 CN2022114449W WO2023065811A1 WO 2023065811 A1 WO2023065811 A1 WO 2023065811A1 CN 2022114449 W CN2022114449 W CN 2022114449W WO 2023065811 A1 WO2023065811 A1 WO 2023065811A1
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- Prior art keywords
- methanol
- headspace
- essential oil
- cigarettes
- signal value
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- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 title claims abstract description 231
- 239000000341 volatile oil Substances 0.000 title claims abstract description 36
- 238000000034 method Methods 0.000 title claims abstract description 35
- 235000019504 cigarettes Nutrition 0.000 title claims abstract description 34
- 239000011324 bead Substances 0.000 title abstract description 6
- 238000003988 headspace gas chromatography Methods 0.000 claims abstract description 11
- 238000009210 therapy by ultrasound Methods 0.000 claims abstract description 4
- 238000001514 detection method Methods 0.000 claims description 25
- 239000007789 gas Substances 0.000 claims description 10
- 238000009834 vaporization Methods 0.000 claims description 10
- 239000001257 hydrogen Substances 0.000 claims description 7
- 229910052739 hydrogen Inorganic materials 0.000 claims description 7
- 238000002347 injection Methods 0.000 claims description 7
- 239000007924 injection Substances 0.000 claims description 7
- 230000008016 vaporization Effects 0.000 claims description 7
- 238000004817 gas chromatography Methods 0.000 claims description 6
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims description 5
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 4
- 238000012546 transfer Methods 0.000 claims description 4
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims description 3
- 239000001301 oxygen Substances 0.000 claims description 3
- 229910052760 oxygen Inorganic materials 0.000 claims description 3
- 239000012086 standard solution Substances 0.000 claims description 3
- 238000003556 assay Methods 0.000 claims description 2
- 239000012159 carrier gas Substances 0.000 claims description 2
- 238000011049 filling Methods 0.000 claims description 2
- 150000002431 hydrogen Chemical class 0.000 claims description 2
- 229910052757 nitrogen Inorganic materials 0.000 claims description 2
- 230000010355 oscillation Effects 0.000 claims 1
- 230000009286 beneficial effect Effects 0.000 abstract description 2
- 238000007789 sealing Methods 0.000 abstract description 2
- 238000000691 measurement method Methods 0.000 abstract 1
- 235000002017 Zea mays subsp mays Nutrition 0.000 description 25
- 241000482268 Zea mays subsp. mays Species 0.000 description 25
- 239000000523 sample Substances 0.000 description 14
- WSFSSNUMVMOOMR-UHFFFAOYSA-N Formaldehyde Chemical compound O=C WSFSSNUMVMOOMR-UHFFFAOYSA-N 0.000 description 6
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 6
- 229910052782 aluminium Inorganic materials 0.000 description 6
- 239000012071 phase Substances 0.000 description 6
- 238000009835 boiling Methods 0.000 description 5
- 238000011067 equilibration Methods 0.000 description 5
- 229920001343 polytetrafluoroethylene Polymers 0.000 description 5
- 239000004810 polytetrafluoroethylene Substances 0.000 description 5
- 235000013305 food Nutrition 0.000 description 4
- 239000003921 oil Substances 0.000 description 4
- 239000003960 organic solvent Substances 0.000 description 4
- 229920001296 polysiloxane Polymers 0.000 description 4
- 230000035945 sensitivity Effects 0.000 description 4
- DNIAPMSPPWPWGF-UHFFFAOYSA-N Propylene glycol Chemical compound CC(O)CO DNIAPMSPPWPWGF-UHFFFAOYSA-N 0.000 description 3
- 230000000694 effects Effects 0.000 description 3
- 239000011521 glass Substances 0.000 description 3
- 150000002500 ions Chemical class 0.000 description 3
- 238000005070 sampling Methods 0.000 description 3
- 239000002904 solvent Substances 0.000 description 3
- WWZKQHOCKIZLMA-UHFFFAOYSA-N Caprylic acid Natural products CCCCCCCC(O)=O WWZKQHOCKIZLMA-UHFFFAOYSA-N 0.000 description 2
- 239000005635 Caprylic acid (CAS 124-07-2) Substances 0.000 description 2
- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 description 2
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 2
- 238000004566 IR spectroscopy Methods 0.000 description 2
- 238000001069 Raman spectroscopy Methods 0.000 description 2
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 2
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Natural products CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 description 2
- 238000011156 evaluation Methods 0.000 description 2
- 238000000605 extraction Methods 0.000 description 2
- 238000004128 high performance liquid chromatography Methods 0.000 description 2
- BDAGIHXWWSANSR-UHFFFAOYSA-N methanoic acid Natural products OC=O BDAGIHXWWSANSR-UHFFFAOYSA-N 0.000 description 2
- 229960002446 octanoic acid Drugs 0.000 description 2
- 239000012488 sample solution Substances 0.000 description 2
- 238000000926 separation method Methods 0.000 description 2
- 239000000741 silica gel Substances 0.000 description 2
- 229910002027 silica gel Inorganic materials 0.000 description 2
- 239000000243 solution Substances 0.000 description 2
- 238000002798 spectrophotometry method Methods 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 238000012360 testing method Methods 0.000 description 2
- OSWFIVFLDKOXQC-UHFFFAOYSA-N 4-(3-methoxyphenyl)aniline Chemical compound COC1=CC=CC(C=2C=CC(N)=CC=2)=C1 OSWFIVFLDKOXQC-UHFFFAOYSA-N 0.000 description 1
- AXDJCCTWPBKUKL-UHFFFAOYSA-N 4-[(4-aminophenyl)-(4-imino-3-methylcyclohexa-2,5-dien-1-ylidene)methyl]aniline;hydron;chloride Chemical compound Cl.C1=CC(=N)C(C)=CC1=C(C=1C=CC(N)=CC=1)C1=CC=C(N)C=C1 AXDJCCTWPBKUKL-UHFFFAOYSA-N 0.000 description 1
- 201000004569 Blindness Diseases 0.000 description 1
- 206010010071 Coma Diseases 0.000 description 1
- BDAGIHXWWSANSR-UHFFFAOYSA-M Formate Chemical compound [O-]C=O BDAGIHXWWSANSR-UHFFFAOYSA-M 0.000 description 1
- 235000014443 Pyrus communis Nutrition 0.000 description 1
- LSNNMFCWUKXFEE-UHFFFAOYSA-N Sulfurous acid Chemical compound OS(O)=O LSNNMFCWUKXFEE-UHFFFAOYSA-N 0.000 description 1
- 239000004809 Teflon Substances 0.000 description 1
- 229920006362 Teflon® Polymers 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 210000003169 central nervous system Anatomy 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- HLVXFWDLRHCZEI-UHFFFAOYSA-N chromotropic acid Chemical compound OS(=O)(=O)C1=CC(O)=C2C(O)=CC(S(O)(=O)=O)=CC2=C1 HLVXFWDLRHCZEI-UHFFFAOYSA-N 0.000 description 1
- 235000019506 cigar Nutrition 0.000 description 1
- 230000007423 decrease Effects 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 238000004090 dissolution Methods 0.000 description 1
- 235000020188 drinking water Nutrition 0.000 description 1
- 239000003651 drinking water Substances 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 238000010812 external standard method Methods 0.000 description 1
- 239000002778 food additive Substances 0.000 description 1
- 235000013373 food additive Nutrition 0.000 description 1
- 235000019253 formic acid Nutrition 0.000 description 1
- 125000000524 functional group Chemical group 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 239000007791 liquid phase Substances 0.000 description 1
- 230000014759 maintenance of location Effects 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 239000011159 matrix material Substances 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- WSFSSNUMVMOOMR-NJFSPNSNSA-N methanone Chemical compound O=[14CH2] WSFSSNUMVMOOMR-NJFSPNSNSA-N 0.000 description 1
- 125000000956 methoxy group Chemical group [H]C([H])([H])O* 0.000 description 1
- 125000002496 methyl group Chemical group [H]C([H])([H])* 0.000 description 1
- 239000003208 petroleum Substances 0.000 description 1
- 238000005375 photometry Methods 0.000 description 1
- 238000002203 pretreatment Methods 0.000 description 1
- 238000010926 purge Methods 0.000 description 1
- 238000011002 quantification Methods 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 238000011084 recovery Methods 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 230000000391 smoking effect Effects 0.000 description 1
- 238000004611 spectroscopical analysis Methods 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- 239000013076 target substance Substances 0.000 description 1
- 125000003944 tolyl group Chemical group 0.000 description 1
- 231100000331 toxic Toxicity 0.000 description 1
- 230000002588 toxic effect Effects 0.000 description 1
- 238000000870 ultraviolet spectroscopy Methods 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 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
- 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
- G01N30/62—Detectors specially adapted therefor
- G01N30/64—Electrical detectors
- G01N30/68—Flame ionisation detectors
Definitions
- the invention relates to the technical field of detection of methanol content, in particular to a method for accurately measuring the content of methanol in popcorn essential oil for cigarettes by using full vaporization headspace gas chromatography.
- Methanol is an important organic raw material and is widely used in industry. Methanol is highly toxic. Once ingested by the human body, it will be metabolized into formic acid and formate that are harmful to the central nervous system. In severe cases, it will cause blindness, coma or even death. Therefore, in food, drinking water and air, the concentration of methanol has strict restrictions and must be below 5-10mg/kg.
- Popcorn essential oil for cigarettes is an important food additive. A large amount of chemical solvents such as ethanol, propylene glycol, and petroleum ether are used in the process of dissolution, extraction, and synthesis. These residual methanol may be brought into food. And then pose a serious threat to human health. In view of this, it is necessary to establish a rapid and accurate method for the determination of residual methanol content in popcorn essential oil for cigarettes, which has an important guiding role in ensuring food quality and reducing safety risks.
- the detection methods of the methanol content in the popcorn essential oil (oil phase) for cigarettes are mainly gas chromatography and high performance liquid chromatography.
- gas chromatography since the popcorn essential oil system for cigarettes contains high-boiling solvents such as caprylic acid glyceride (boiling point is 456 ° C), direct sampling detection will pollute the sampling system, and then affect the service life of the instrument; therefore, in order to reduce Risk, pretreatment steps such as extraction and separation with organic solvents are required before detection. These pretreatments are not only cumbersome and inefficient, but also affect the accuracy of detection results.
- Raman spectroscopy, infrared spectroscopy, and ultraviolet-visible spectroscopy are based on the determination of the characteristic peaks of the characteristic functional groups (methyl) in methanol to determine the methanol content.
- the main problem is that it will be affected by the complex matrix of the sample and the detection sensitivity is not high.
- the principle of spectrophotometric method for measuring methanol is to oxidize methanol into formaldehyde, and formaldehyde reacts with chromogenic agents such as sulfite fuchsin, chromotropic acid, etc.
- the present invention is proposed to solve the above-mentioned problems.
- the present invention provides a method for accurately measuring the content of methanol in popcorn essential oil system for cigarettes by using full vaporization headspace gas chromatography.
- the method of the invention has the advantages of fast detection speed, high result accuracy, simple and convenient operation, etc., and overcomes the disadvantages existing in the current determination of the methanol content in the oil phase system.
- the present invention adopts full-vaporization headspace gas chromatography to measure the methanol content in the popcorn essential oil for cigarettes.
- the specific principle is: in a closed headspace bottle, when the equilibrium temperature of the headspace exceeds the boiling point of methanol, The methanol will be completely transferred from the liquid phase to the gas phase; the signal value of methanol is determined based on full vaporization headspace gas chromatography, and then the methanol content in the popcorn essential oil for cigarettes is calculated through the standard curve.
- the present invention realizes through following technical scheme:
- a method for accurately measuring the content of methanol in the popcorn essential oil for cigarettes by full-vaporized headspace gas chromatography comprising the steps of:
- the puffed pearl essential oil for cigarettes into a headspace bottle after ultrasonic treatment and seal it;
- the conditions for ultrasonic treatment are preferably: 400w, time: 5min;
- the puffed pear essential oil for cigarettes can be liquid;
- step 2 Place the headspace vial of step 1 in the headspace sampler, and measure the signal value of methanol in the headspace vial by full vaporization headspace gas chromatography;
- the eluting time of the methanol peak is 0.668 min.
- the conditions of the headspace sampler in step 2 are as follows: the initial equilibrium temperature is 105°C, the equilibrium time is 2min; The time to GC is 20s; the maximum injection volume is 40 ⁇ L.
- gas chromatography operating conditions in step 2 hydrogen flame ion detector, carrier gas is nitrogen, flow rate is 25mL/min; combustible gas is hydrogen, flow rate is 30mL/min; assisted gas is oxygen, flow rate is 400mL/min;
- the detector temperature is 250°C, the split ratio is 2:1, and the detection time is 2min.
- A is -157.66 ⁇ 21.91; B is 83.99 ⁇ 0.9197.
- the method of the present invention utilizes full-vaporized headspace gas chromatography to measure the methanol content in the popcorn essential oil for cigarettes for the first time.
- the detection method of the invention is easy to operate and has high precision; the limit of quantification of methanol detection in the popcorn essential oil for cigarettes can reach 0.73 mg/mL.
- the detection method of the invention can detect in batches, thereby improving the efficiency; it overcomes the disadvantages of low detection sensitivity, cumbersome operation, low time-consuming efficiency, high organic solvent loss and the like in the prior art method.
- the method of the present invention utilizes full-vaporized headspace gas chromatography to accurately measure the methanol content in the popcorn essential oil for cigarettes, avoids the influence of high-boiling solvents on the measurement results during direct sample injection, and has a wide range of applications.
- the method of the present invention can accurately quantitatively analyze the methanol content in the popcorn essential oil for cigarettes, provide guidance for the determination of the methanol content in the oil phase, and play an important guiding role in ensuring food quality and reducing safety risks.
- Fig. 1 is the gas chromatogram of the volatile target substance in the popcorn essential oil for smoking with the temperature of the chromatographic column being 60°C.
- Figure 2 is a graph showing the effect of headspace equilibration time on methanol signal value.
- Fig. 3 is a graph showing the effect of the headspace equilibrium temperature on the methanol signal value.
- Equipment and reagents used DANI HS 86.50 PLUS, Italy type automatic headspace sampler, Agilent GC 8860, US type gas chromatograph (hydrogen flame ion detector, GS-Q type capillary column), headspace bottle ( 20.0ml), blue Teflon/blue silicone septa (with aluminum cap).
- the headspace sampler conditions were as follows:
- the equilibrium temperature is 105°C
- the equilibrium time is 2min
- the pressurization time of the headspace bottle is 15s
- the depressurization time is 15s
- the filling time of the quantitative loop is 10s
- the transfer line time is 20s
- the injection purge time is 20s
- the pressurization pressure is 1bar.
- the inlet pressure is 22.47psi
- the inlet temperature is 250°C
- the split ratio is 2:1
- the detector temperature is 250°C
- the detection time is 2min
- the hydrogen flow rate is 30mL /min
- the oxygen flow rate of the assisted gas is 400mL/min
- the make-up flow is 25mL/min
- the detector temperature is 250°C.
- FIG. 1 is a gas chromatogram of a sample of cigar bead extract when the oven temperature is 60°C. It can be seen from Figure 1 that methanol and other volatile substances can be better separated at a lower oven temperature, and the methanol retention time is 0.668min. Therefore, the temperature of the chromatographic column selected in the present invention is 60°C.
- A is the GC signal value (ie peak area) of methanol in the headspace vial
- C is the concentration of methanol in the standard solution (unit: mg/mL).
- the limit of quantitation (LOQ) of methanol detection by this method can be calculated by the following formula:
- a, s, and ⁇ a are the intercept, slope, and standard deviation of the intercept in formula (1), respectively. From the formula (2), it can be calculated that the quantitative limit of the method for the detection of methanol in the popcorn essential oil for cigarettes is 0.73 mg/mL.
- the reproducibility evaluation of the method of the present invention is to carry out 3 repeated experiments on 4 different paper samples, and compare the detection results to obtain the relative standard deviation value of the detection results.
- the reproducibility test results of the method of the present invention are shown in Table 2. It can be seen from Table 2 that the relative standard deviations of the method for different samples of popcorn essential oil for cigarettes are all less than 3.89%. Therefore, it can be considered that the method of the present invention has good reproducibility for detecting residual methanol in the popcorn essential oil for cigarettes.
- the accuracy evaluation of the method of the present invention is to add 10-80 ⁇ L of pure methanol solution to 10mL sample (methanol content in the sample is 1.94mg/mL), respectively, to obtain a spiked sample solution.
- the non-spiked popcorn essential oil sample with a methanol content of 1.94 mg/mL was used as a reference object to detect the net contribution of the added standard, and the results are shown in Table 3. It can be seen from Table 3 that the recovery rate of the method of the present invention for detecting the methanol content in the popcorn essential oil for cigarettes is between 97.8% and 101%, which shows that the method has good accuracy.
- the method of the present invention can accurately quantitatively analyze the methanol content in the popcorn essential oil for cigarettes; the detection method is easy to operate and has high precision.
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- 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)
- Other Investigation Or Analysis Of Materials By Electrical Means (AREA)
- Sampling And Sample Adjustment (AREA)
Abstract
Procédé de mesure de la teneur en méthanol dans une huile essentielle de bille à éclater de cigarette à l'aide d'un procédé de chromatographie en phase gazeuse d'espace de tête entièrement vaporisé, comprenant les étapes suivantes consistant : (1) après soumission de l'huile essentielle de bille à éclater de cigarette à un traitement par ultrasons, à mettre en place l'huile essentielle de bille à éclater de cigarette dans une bouteille d'espace de tête et à refermer hermétiquement ; (2) à mettre en place la bouteille d'espace de tête de l'étape (1) dans un injecteur d'échantillon d'espace de tête, et à mesurer une valeur de signal du méthanol dans la bouteille d'espace de tête au moyen d'un procédé de chromatographie en phase gazeuse d'espace de tête entièrement vaporisé ; et (3) à substituer la valeur de signal du méthanol obtenu à l'étape (2) dans une courbe standard afin d'obtenir la teneur en méthanol dans l'huile essentielle de bille à éclater de cigarette. L'effet bénéfique est que le procédé de mesure est simple et pratique à utiliser et d'une grande précision.
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CN202111232950.3A CN113960229A (zh) | 2021-10-22 | 2021-10-22 | 一种烟用爆珠精油中甲醇含量的测定方法 |
CN202111232950.3 | 2021-10-22 |
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CN102520082A (zh) * | 2011-12-01 | 2012-06-27 | 湖南省湘维有限公司 | 用全蒸发顶空气相色谱法测定聚乙烯醇中的挥发性组分的方法 |
CN102680596A (zh) * | 2012-05-07 | 2012-09-19 | 广东中烟工业有限责任公司 | 一种烟用胶黏剂中有机挥发性物质的检测方法 |
JP2014044175A (ja) * | 2012-08-28 | 2014-03-13 | Shimadzu Corp | 親水性化合物の分析方法 |
CN103512994A (zh) * | 2013-10-14 | 2014-01-15 | 福建中烟工业有限责任公司 | 一种测定烟用滤棒中挥发性成分残留的方法 |
CN107515260A (zh) * | 2017-08-16 | 2017-12-26 | 重庆大学 | 一种绝缘油中甲醇含量的测定方法 |
CN113960229A (zh) * | 2021-10-22 | 2022-01-21 | 云南中烟工业有限责任公司 | 一种烟用爆珠精油中甲醇含量的测定方法 |
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