CN108760924B - Method for extracting and detecting characteristic components of fragrant threads and popping beads of filter sticks - Google Patents
Method for extracting and detecting characteristic components of fragrant threads and popping beads of filter sticks Download PDFInfo
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Abstract
A method for extracting and detecting characteristic components of aromatic threads and bead explosion of filter sticks belongs to the field of detection of tobacco materials, and comprises the following steps: dispersing a sample to be detected and analyzed by distilled water, carrying out centrifugal treatment, adding inorganic salt into filtrate, then placing the filtrate into a double-layer composite bag, adding an organic solvent, carrying out 50-900W ultrasonic treatment, taking out an organic phase, and carrying out qualitative and quantitative analysis on characteristic components by using gas chromatography-mass spectrometry. The method can be applied to enrichment, separation and extraction of characteristic components such as cigarette filter stick incense stick, exploded bead and the like. Compared with the traditional extraction separation method, the enrichment method is quicker, simpler, more convenient, lower in temperature and green, and has important significance for improving the product quality.
Description
Technical Field
The invention belongs to the field of detection of tobacco materials, and particularly relates to a method for extracting and detecting characteristic components of filter stick fragrant threads and popping beads.
Background
With the increase of international cigarette inhibition calls and the increasing concern of cigarette consumers on self health, the low-tar and low-harm cigarette becomes the mainstream of cigarettes in the future world, but the harm and tar reduction is accompanied with the loss of cigarette aroma and the deterioration of comfort. At present, in addition to the defect of making up for the fragrance of cigarettes by adding tobacco essence to conventional tobacco shreds, the flavoring of the filter tip also becomes one of important flavoring modes of the cigarettes, and the filter tip cigarette with a special specification is formed by flavoring the filter tip. The special-specification filter stick cigarette mainly refers to cigarettes containing bead blasting filter sticks, fragrant line filter sticks and the like. The volatile flavor components in the exploded bead and the incense stick play an important role in the quality of cigarettes.
Therefore, establishing a method for enriching, separating and extracting trace volatile aroma components in cigarette filter sticks (filter stick aroma lines and exploded beads) with special specifications has important significance for improving and monitoring the quality of cigarette products. In recent years, the following methods are mainly used for characteristic components in different samples:
(1) liquid-liquid extraction method
The liquid-liquid extraction method is a traditional separation method, also called solvent extraction separation method. The liquid-liquid extraction has the advantages of simple equipment and quick operation. The disadvantages are time consuming, high workload and limited application because the extraction solvent is often a volatile, flammable and toxic substance.
Static headspace method and dynamic blow-catch method
Headspace method is a method of extracting the analyte from the sample using air, nitrogen, helium or other gases. It is divided into two methods, namely a static headspace method (HS) and a dynamic blowing and catching method (purge & trap, P & T). Is suitable for extracting volatile components with the boiling point lower than 200 ℃ from liquid or solid samples, and is widely applied to food and environmental monitoring departments and the like. The method has the advantages of simple operation, and is suitable for extracting volatile substances in liquid samples, viscous bodies and even solids, especially the compounds with the boiling point lower than 125 ℃. The disadvantage is that the method is not capable of concentrating volatile components, so the method has low sensitivity and is only suitable for components with high volatility; in addition, since the extraction is carried out under static equilibrium conditions, the volatile components in the sample cannot be extracted completely, and therefore, the different substances in different substrates need to be carefully calibrated for quantification. However, the quantitative reproducibility was not good.
(3) Simultaneous distillation and extraction
Meanwhile, distillation extraction is an efficient extraction method for volatile components. Its advantages are high concentrating power to volatile organic components thousands of times, and simple operation. The method has the disadvantages that a large amount of solvent is needed in the pretreatment process, certain pollution is caused to the environment, the heating time is long, and the characteristic components in the sample are easy to change in the heating process.
Solid phase extraction
Solid Phase Extraction (SPE) is an extraction method developed by combining a similar phase dissolution mechanism of substance interaction and the basic principle of HPLC and GC stationary phases. At present, the method is mainly applied to analysis of organic substances such as polycyclic aromatic hydrocarbon and polychlorinated biphenyl in water, pesticide and herbicide residue analysis in fruits, vegetables and foods, antibiotic analysis, clinical drug analysis and the like. SPE has the characteristics of small solvent consumption, convenience, safety, high efficiency and the like. The method has the disadvantages that the pretreatment method is complex, and most pretreatment processes need a large amount of solvent, thereby causing certain pollution to the environment.
The ultrasonic-assisted liquid-liquid extraction utilizes the mechanical effect, the cavitation effect and the thermal effect of ultrasonic waves, increases the penetrating power of a medium by increasing the movement speed of medium molecules, realizes low-temperature to normal-temperature extraction through a low-temperature system carried by the ultrasonic, simultaneously assists the liquid-liquid extraction of an organic solvent, and is carried out in a closed system in the whole extraction process, so that the solvent is not volatilized, the liquid-liquid extraction is green and environment-friendly, and the low-temperature rapid extraction is realized. At present, no report related to enrichment and separation of special filter stick characteristic components by ultrasonic-assisted liquid-liquid extraction is found.
Disclosure of Invention
The invention aims to overcome the technical defect that the pretreatment of the existing characteristic components is complex, and provides a low-temperature and rapid enrichment and extraction method for the characteristic components of cigarette filter stick flavor threads and exploded beads by means of a combined technology of ultrasonic-assisted liquid-liquid extraction. The invention also provides a method for detecting the characteristic components of the fragrant threads and the popping beads of the filter stick.
A method for extracting characteristic components of filter stick incense threads and popping beads comprises the following steps: dispersing samples such as filter stick aroma lines or exploded beads and the like with a certain proportion of water, centrifuging by a centrifuge to remove solid matters or directly leaving a certain volume of water, adding a certain amount of inorganic salt, placing the aqueous solution of the inorganic salt in a double-layer composite bag, adding a certain amount of organic solvent, placing the double-layer composite bag in a low-temperature ultrasonic extractor after heat sealing, carrying out ultrasonic treatment at 50-900W for 1.0-50.0min at 5-25 ℃, taking out the organic phase, and qualitatively and quantitatively analyzing characteristic components in the filter stick by adopting gas chromatography-mass spectrometry.
Specifically, the solvent may be one or more of petroleum ether, n-hexane, dichloromethane, diethyl ether and methyl tert-butyl ether. The dosage of the organic solvent for every two incense threads or two exploded beads is 0.5-10.0 mL.
The inorganic salt is one or more of sodium chloride, potassium chloride, sodium sulfate and potassium sulfate, and the amount of the inorganic salt is 3.0-10.0g for every two incense threads or two exploded beads. The dosage of every two aromatic threads or two bead blasting water is 10-100 mL, preferably 10-25 mL.
Gas chromatography conditions:
a chromatographic column: HP-5MS (60 m.times.0.25 mm.times.0.25 μm);
sample inlet temperature: 280 ℃;
carrier gas: helium, column flow rate of 1.0mL/min
The split ratio is as follows: 5: 1, the sampling amount is 1.0 mu L;
temperature programming: 50 deg.C (for 2 min), 4 deg.C/min to 280 deg.C (for 20 min).
Mass spectrum conditions:
electron bombardment of the ion source (EI) with electron current of 70 eV; the ion source temperature is 230 ℃, the quadrupole rod temperature is 150 ℃, and the transmission line temperature is 280 ℃; selecting ion scanning; the characteristic component selection scan ion and retention time are shown in table 1.
Table 1 selection of scan ions and retention times for each feature
Preparing an internal standard solution and a standard working solution:
weighing 0.05g of phenol acetate in a 25mL volumetric flask, fixing the volume to the scale with dichloromethane, and shaking up to obtain an internal standard stock solution with the internal standard concentration of 2.0 mg/mL; and transferring 200 mu L of internal standard stock solution into a 50mL volumetric flask, using dichloromethane to fix the volume to the scale, and shaking up to obtain the internal standard solution with the internal standard concentration of 8 mu g/mL.
Weighing 0.05g of ethyl butyrate, isoamyl acetate, limonene, linalool, L-menthone, menthol and linalyl acetate in a 50mL volumetric flask respectively, and fixing the volume to a scale by using an internal standard solution to obtain a mixed standard stock solution; transferring 300 mu L of mixed standard stock solution into a 10mL volumetric flask, using an internal standard solution to perform constant volume to a scale to obtain mixed standard working mother solution, and then diluting to obtain standard working solution with the concentrations of ethyl butyrate, isoamyl acetate, limonene, linalool, L-menthone, menthol and linalool acetate of 30 mu g/mL, 15 mu g/mL, 6 mu g/mL, 3 mu g/mL, 1.5 mu g/mL and 0.3 mu g/mL.
And drawing a standard working curve of each characteristic component by taking the ratio of the chromatographic peak areas of each standard solution and the phenol acetate as the ordinate and the concentration of the standard solution corresponding to each characteristic component as the abscissa. And calculating to obtain a standard curve regression equation, and then respectively substituting the ratios of the chromatographic peak areas of the characteristic components detected in the sample solution and the phenol acetate into the corresponding standard curve regression equations to obtain the content of the characteristic components, wherein the specific results are shown in table 2.
TABLE 2 Linear equation, detection limit and recovery rate of each characteristic component
Effects of the invention
The method can be applied to enrichment, separation and extraction of characteristic components such as cigarette filter stick incense stick, exploded bead and the like. Compared with the traditional extraction separation method, the enrichment method is quicker, simpler, more convenient, lower in temperature and green, and has important significance for improving the product quality.
The method comprises the steps of controlling other pretreatment conditions to be unchanged for the same bead blasting (filter stick flavor line), extracting characteristic components in the bead blasting by adopting two modes of adding inorganic salt into a water phase and not adding the inorganic salt, then carrying out GC-MS analysis, and carrying out quantitative analysis on the characteristic components. The results show that: after addition of inorganic salts to the aqueous phase, a higher content of the characteristic components in the popped beads (filter stick threads) was detected than in the pure aqueous phase, which is probably due to the fact that the addition of inorganic salts to the aqueous phase reduces the solubility of the characteristic components in the aqueous phase, which is more favorable for the extraction of the characteristic components by the organic phase.
Drawings
FIG. 1 is a chromatogram of a standard working solution of the present invention, in which ethyl butyrate 1, isoamyl acetate 2, limonene 3, phenol acetate 4, linalool 5, L-menthone 6, menthol 7, linalyl acetate 8.
Detailed Description
The technical solution of the present invention is further described in detail below with reference to specific examples and comparative examples, but the scope of the present invention is not limited thereto.
In the following examples where gas chromatography-mass spectrometry was used for detection,
gas chromatography conditions:
a chromatographic column: HP-5MS (60 m.times.0.25 mm.times.0.25 μm);
sample inlet temperature: 280 ℃;
carrier gas: helium, column flow rate of 1.0mL/min
The split ratio is as follows: 5: 1, the sampling amount is 1.0 mu L;
temperature programming: 50 deg.C (for 2 min), 4 deg.C/min to 280 deg.C (for 20 min).
Mass spectrum conditions:
electron bombardment of the ion source (EI) with electron current of 70 eV; the ion source temperature is 230 ℃, the quadrupole rod temperature is 150 ℃, and the transmission line temperature is 280 ℃; selecting ion scanning; compound selection scan ion and retention times are shown in table 3.
Table 3 characteristic component selection scan ion and retention time
Example 1
A method for extracting characteristic components of filter stick bead explosion comprises the following steps:
taking 2 filter stick blasting beads, mashing the filter stick blasting beads in a mortar, adding 100mL of distilled water, fully stirring, filtering to 10mL, placing the filter stick blasting beads in a double-layer composite bag, adding 3g of sodium chloride, adding 1.0mL of n-hexane, placing the double-layer composite bag in a low-temperature ultrasonic extractor after heat sealing, carrying out ultrasonic treatment of 500W at the treatment temperature of 5 ℃ for 5min, then taking out the n-hexane phase, analyzing the n-hexane phase by adopting gas chromatography-mass spectrometry, carrying out quantitative determination by applying an internal standard curve method, and determining the main characteristic components in the filter stick blasting beads: ethyl butyrate (18.23. mu.g/g), isoamyl acetate (9.36. mu.g/g), limonene (15.34. mu.g/g), linalool (5.39. mu.g/g), L-menthone (11.69. mu.g/g), menthol (21.93. mu.g/g), linalyl acetate (4.89. mu.g/g) and the like.
Comparative example 1
Taking three parts of filter stick blasting beads, 2 particles of each part, mashing in a mortar, adding 10mL of distilled water and 1mL of n-hexane into the first part, adding 3g of sodium chloride and 10mL of distilled water into the second part, adding 10.0g of sodium chloride and 1.0mL of n-hexane into the third part, then placing the third part in a low-temperature ultrasonic extractor, carrying out ultrasonic treatment at 500W for 5min at the treatment temperature, blowing the extraction solution extracted by the sodium chloride and the distilled water to dry by using a nitrogen blowing instrument, and then adding 10mL of ethanol for redissolution; extracting a sample with n-hexane, and taking out a n-hexane phase; then the hexane phase and ethanol phase are filtered through organic filter membranes, gas chromatography-mass spectrometry is adopted for analysis, and an internal standard curve method is applied for quantitative determination, wherein the results are shown in table 4:
TABLE 4 comparison table of characteristic components in bead blasting for three cases
It can be seen from table 4 that the extraction effect of water and n-hexane is better than that of water and inorganic salt, and the extraction effect of salt and n-hexane is better than that of water and n-hexane, as can be seen from comparative example 1, the extraction effect of the three compounded is the best, mainly because the distilled water increases the contact area between the characteristic component in the exploded bead and the organic phase, the inorganic salt reduces the solubility of the characteristic component in the distilled water, the characteristic component in the filter stick flavor line is more effectively provided through the extraction of the organic solvent n-hexane, and the GC/MS analysis can be directly performed.
Example 2
A method for extracting characteristic components of a filter stick incense stick comprises the following steps:
taking 2 filter stick incense threads (about 28cm), adding 100mL of distilled water, fully stirring, filtering to 25mL, placing a sample in a double-layer composite bag, adding 8g of potassium chloride, adding 1.5 mL of dichloromethane, placing the double-layer composite bag in a low-temperature ultrasonic extractor after heat sealing, carrying out ultrasonic treatment at 350W for 5min at the treatment temperature of 10 ℃, then taking out a dichloromethane phase, analyzing the dichloromethane phase by adopting gas chromatography-mass spectrometry, and quantitatively determining by using an internal standard curve method that the filter stick incense threads contain characteristic components such as linalool (15.25 mu g/g), L-menthone (20.96 mu g/g), menthol (18.37 mu g/g) and the like.
Comparative example 2
Taking three parts of 2 aromatic filter stick threads, adding 25mL of distilled water and 1.5 mL of dichloromethane into the first part, adding 8g of potassium chloride and 25mL of distilled water into the second part, adding 8g of potassium chloride and 1.5 mL of dichloromethane into the third part, then placing the mixture into a low-temperature ultrasonic extraction instrument, carrying out ultrasonic treatment by 350W at the treatment temperature of 10 ℃ for 5min, blowing the extraction solution extracted by the potassium chloride and the distilled water by a nitrogen blowing instrument for drying, and then adding 10mL of ethanol for redissolution; extracting a sample by using dichloromethane, and taking out a dichloromethane phase; then the dichloromethane phase and the ethanol phase pass through an organic filter membrane, the analysis is carried out by adopting gas chromatography-mass spectrometry, the quantitative determination is carried out by applying an internal standard curve method, and the results are shown in the table 5:
TABLE 5 comparison table of characteristic components in three cases of extraction filter stick incense
As can be seen from table 5, the extraction effect of water and dichloromethane is better than that of water and inorganic salt, and the extraction effect of salt and dichloromethane is better than that of water and dichloromethane, as can be seen from comparative example 2, the extraction effect of the compound of the three is the best, mainly because the distilled water increases the contact area between the characteristic components in the filter stick incense thread and the organic phase, the inorganic salt reduces the solubility of the characteristic components in the distilled water, the characteristic components in the filter stick incense thread are more effectively extracted through the extraction of the organic solvent dichloromethane, and the GC/MS analysis can be directly performed.
The foregoing is illustrative of only a few specific embodiments in which the invention may be practiced. It is obvious that the invention is not limited to the above embodiments, but that many variations are possible. All modifications which can be derived or suggested by a person skilled in the art from the disclosure of the present invention are to be considered within the scope of the invention.
Claims (2)
1. A method for detecting characteristic components of filter stick incense threads and popping beads is characterized by comprising the following steps: dispersing a sample to be detected and analyzed by distilled water, performing centrifugal treatment, adding inorganic salt into filtrate, then placing the filtrate into a double-layer composite bag, adding an organic solvent, performing 50-900W ultrasonic treatment, taking out an organic phase, and performing qualitative and quantitative analysis on characteristic components by using a gas chromatography-mass spectrometry, wherein the quantitative analysis adopts an internal standard curve method, and the characteristic components are ethyl butyrate, isoamyl acetate, limonene, linalool, L-menthone, menthol and linalyl acetate; the organic solvent is n-hexane or dichloromethane, and the dosage of every two aromatic threads or two bead blasting organic solvents is 0.5-10.0 mL; the used inorganic salt is sodium chloride, the dosage of every two incense threads or two bead blasting inorganic salts is 3.0-10.0g, the dosage of every two incense threads or two bead blasting water is 10-100 mL, and the gas chromatography conditions are as follows:
a chromatographic column: HP-5MS 60 m × 0.25 mm × 0.25 μm;
sample inlet temperature: 280 ℃;
carrier gas: helium, column flow rate of 1.0mL/min
The split ratio is as follows: 5: 1, the sample injection amount is 1.0 mu L;
temperature programming: keeping at 50 deg.C for 2min, increasing the temperature to 280 deg.C at 4 deg.C/min and keeping at 280 deg.C for 20 min;
mass spectrum conditions:
bombarding an ion source by electrons, wherein the electron current is 70 ev; the ion source temperature is 230 ℃, the quadrupole rod temperature is 150 ℃, and the transmission line temperature is 280 ℃; an ion scan is selected.
2. The method for detecting the characteristic components of the filter stick incense stick and the popping beads as claimed in claim 1, wherein the ultrasonic temperature is 5-25 ℃, and the ultrasonic treatment time is 1-50 min.
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| CN109696494A (en) * | 2018-12-17 | 2019-04-30 | 云南中烟工业有限责任公司 | A method of measuring 7 kinds of colorants in quick-fried pearl |
| CN109856257A (en) * | 2018-12-26 | 2019-06-07 | 广东中烟工业有限责任公司 | A kind of determination method of volatile fragrant components and its application |
| CN110426468A (en) * | 2019-07-31 | 2019-11-08 | 甘肃烟草工业有限责任公司 | The extracting process and application of a kind of cigarette with quick-fried pearl (capsule) sample |
| CN112763595A (en) * | 2020-12-16 | 2021-05-07 | 河南中烟工业有限责任公司 | Method for detecting inclusion of bead blasting for cigarettes |
| CN112924609B (en) * | 2021-01-29 | 2023-02-03 | 福建中烟工业有限责任公司 | Method for analyzing volatile aroma components contained in bead blasting filter stick |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102072940A (en) * | 2010-11-11 | 2011-05-25 | 中国烟草总公司湖北省公司 | Method for measuring contents of coumarin and safrole in flavor and fragrance for cigarette |
| CN102128897A (en) * | 2010-12-08 | 2011-07-20 | 江南大学 | Ultrasound-assisted emulsification-microextraction method for pretreatment of artificially synthesized musk in water body |
| CN104062369A (en) * | 2014-06-19 | 2014-09-24 | 浙江大学 | Method for detecting chlorobenzene in sludge through ultrasonic assisted dispersive liquid-liquid microextraction-gas chromatography |
| CN107064399A (en) * | 2016-12-26 | 2017-08-18 | 上海烟草集团有限责任公司 | A kind of assay method of musk xylene in tobacco additive and sesamol |
Family Cites Families (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US9759705B1 (en) * | 2016-03-09 | 2017-09-12 | King Fahd University Of Petroleum And Minerals | Automated dispersive liquid-liquid microextraction technique for the analysis of N-nitrosamines in water |
-
2018
- 2018-05-31 CN CN201810549419.0A patent/CN108760924B/en active Active
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102072940A (en) * | 2010-11-11 | 2011-05-25 | 中国烟草总公司湖北省公司 | Method for measuring contents of coumarin and safrole in flavor and fragrance for cigarette |
| CN102128897A (en) * | 2010-12-08 | 2011-07-20 | 江南大学 | Ultrasound-assisted emulsification-microextraction method for pretreatment of artificially synthesized musk in water body |
| CN104062369A (en) * | 2014-06-19 | 2014-09-24 | 浙江大学 | Method for detecting chlorobenzene in sludge through ultrasonic assisted dispersive liquid-liquid microextraction-gas chromatography |
| CN107064399A (en) * | 2016-12-26 | 2017-08-18 | 上海烟草集团有限责任公司 | A kind of assay method of musk xylene in tobacco additive and sesamol |
Non-Patent Citations (5)
| Title |
|---|
| Determination of volatile components of saffron by optimized ultrasound-assisted extraction in tandem with dispersive liquid-liquid microextraction followed by gas chromatography-mass spectrometry;Hassan Sereshti 等;《Food Chemistry》;20140115;第143卷;第499-505页 * |
| Rapid Extraction of Imidacloprid in Tomatoes by Ultrasonic Dispersion Liquid–Liquid Microextraction Coupled with LC Determination;Fengxia Qiao 等;《Chromatographia》;20100618;第72卷(第3/4期);第331-335页 * |
| 分散液液微萃取/气相色谱-质谱法同时测定烟用添加剂中8种烷基苯类香味有害物;朱晓兰;《分析测试学报》;20120331;第31卷(第3期);第351-354页 * |
| 超声辅助液液萃取-气相色谱-质谱指纹图谱应用于烟用香精香料的检测;杨君 等;《理化检验（化学分册）》;20121231;第48卷(第5期);第559-562页 * |
| 超声辅助液液萃取法提取烟用香精成分的研究_超声辅助液液萃取法提取烟用香精成分的研究;曲国福 等;《分析实验室》;20071130;第26卷(第11期);第57-60页 * |
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