CN103884622A - Method for determining total quantity of petroleum ether extract from tobacco and tobacco products - Google Patents
Method for determining total quantity of petroleum ether extract from tobacco and tobacco products Download PDFInfo
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- CN103884622A CN103884622A CN201410155174.5A CN201410155174A CN103884622A CN 103884622 A CN103884622 A CN 103884622A CN 201410155174 A CN201410155174 A CN 201410155174A CN 103884622 A CN103884622 A CN 103884622A
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Abstract
The invention provides a method for determining the total quantity of a petroleum ether extract from tobacco and tobacco products. The method comprises the following steps: (A) mixing tobacco or tobacco products with the mass of m0 with petroleum ether, and extracting by an accelerated solvent extraction instrument so as to obtain an extract liquor; and (B) removing a solvent from the extract liquor by rotation evaporation so as to obtain the petroleum ether extract with the mass of m, and calculating the total quantity of the petroleum ether extract from the tobacco or tobacco products. Compared with the prior art, the method adopts the combined techniques of accelerated solvent extraction and reduced pressure distillation to determine the total quantity of the petroleum ether extract from tobacco or tobacco products, and has the advantages of short sample treatment time, high sample detection quantity and high efficiency.
Description
Technical field
The invention belongs to and detect analytical applications technical field, relate in particular to the assay method of tobacco and tobacco product PetroChina Company Limited. ether extract total amount.
Background technology
The key distinction of tobacco and other effects is that tobacco is the raw material of cigarette industry, but not directly eats product.The quality of tobacco is the combined reaction of consumer to the rear flue gas characteristic of tobacco leaf burning, it is good that what the degree that is accepted was high be quality, that summarizes says, to be consumer burn and suck the comprehensive impression of several principal elements and the comprehensive evaluations of smoking security such as the fragrance that produces in process, strength, jealous, pungency to tobacco leaf to quality of tobacco, generally includes two aspects of presentation quality and inherent quality.Inherent quality refers to quality and the security of the flue gas quality such as fragrance when the quantity of various chemical compositions in tobacco leaf and harmony, tobacco leaf burn and suck, jealous, strength, pungency.
The content of main chemical compositions and ratio thereof in tobacco leaf, determined the flue gas characteristic of tobacco and goods thereof to a great extent, thereby directly affect the quality of quality of tobacco.The chemical composition of tobacco leaf is very complicated, sums up and can be divided into three major types: non-nitrogen-containing compound, nitrogen-containing compound and expansion material.Non-nitrogen-containing compound comprises monosaccharide and disaccharide, starch, organic acid, phenols, lipid compound, phytosterin compound, terpenoid, cellulose and pectic substance etc.The fragrance matter of tobacco just comprises organic acid, phenols.Lipid, sterols and terpenoid, it not only has material impact to tobacco flavor, and their conversion, catabolite also are mostly aroma components.
For tobacco lipid compound, after usually extracting with sherwood oil, study.Ligroin extraction mainly contains two large class materials: a class is volatile oil component, comprises a large amount of low-molecular-weight hydro carbons, alcohols, acids, aldehydes, ketone, ester class, low molecule terpene etc.; Another kind of is high molecular lipid, comprises grease, lipoid, sterol, terpene etc.
In summary, tobacco leaf Content of Petroleum Ether Extract is relevant with the perfume quantity of tobacco, in tobacco leaf maturation, modulation, ageing with burn and suck in process, form flavor matter through a series of decomposition, Elopichthys bambusa words, produce fragrance, follow, ligroin extraction Chang Zuowei weighs the important indicator of quality of tobacco and fragrance.
At present, the detection method of tobacco ligroin extraction has the soxhlet extraction of industry standard and the near infrared spectrum detection method of research in recent years, but all has long, the shortcoming such as efficiency is low detection time.
Summary of the invention
In view of this, the technical problem to be solved in the present invention is to provide one to grow tobacco and the assay method of tobacco product PetroChina Company Limited. ether extract total amount.
The invention provides one and grow tobacco and the assay method of tobacco product PetroChina Company Limited. ether extract total amount, comprising:
A) be m by quality
0tobacco or tobacco product mix with sherwood oil, extract by accelerated solvent extraction, be extracted liquid;
B) described extract is removed to desolventizing by decompression distillation, obtain the ligroin extraction that quality is m;
Calculate tobacco or tobacco product PetroChina Company Limited. ether extract total amount.
The present invention also provides one to grow tobacco and the assay method of tobacco product PetroChina Company Limited. ether extract total amount, comprising:
A ') be m by quality
0tobacco or tobacco product mix with sherwood oil, extract by accelerated solvent extraction, be extracted liquid;
B ') described extract is removed to desolventizing by decompression distillation, obtain the ligroin extraction that quality is m;
C ') sherwood oil is removed to desolventizing by decompression distillation, the extract quality obtaining in sherwood oil is m '; The quality of described sherwood oil and steps A ') in sherwood oil used identical in quality;
Calculate tobacco or tobacco product PetroChina Company Limited. ether extract total amount.
The present invention also provides one to grow tobacco and the assay method of tobacco product PetroChina Company Limited. ether extract total amount, comprising:
A 〞) massfraction of measuring moisture in tobacco or tobacco product is ω H
2o;
B 〞) be m by quality
0tobacco or tobacco product mix with sherwood oil, extract by accelerated solvent extraction, be extracted liquid;
C 〞) described extract is removed to desolventizing by decompression distillation, obtain the ligroin extraction that quality is m;
D 〞) by step B 〞) in the sherwood oil of equal quality remove desolventizing by decompression distillation, the extract quality obtaining in sherwood oil is m '; The quality of described sherwood oil and step B 〞) in sherwood oil used identical in quality;
Calculate tobacco or tobacco product PetroChina Company Limited. ether extract total amount.
Preferably, described extraction also adds drying agent.
Preferably, the pressure of described extraction is 5～15MPa; The temperature of extraction is 50 ℃～75 ℃.
Preferably, the temperature of described decompression distillation is 30 ℃～40 ℃.
The invention provides one and grow tobacco and the assay method of tobacco product PetroChina Company Limited. ether extract total amount, comprising: A) be m by quality
0tobacco or tobacco product mix with sherwood oil, extract by accelerated solvent extraction, be extracted liquid; B) described extract is removed to desolventizing by rotary evaporation, obtain the ligroin extraction that quality is m; Calculate tobacco or tobacco product PetroChina Company Limited. ether extract total amount.Compared with prior art, the present invention utilizes accelerated solvent to extract and combines with reduced pressure distillation technique, measures the total amount of tobacco and tobacco product PetroChina Company Limited. ether extract, has the sample preparation time short, and sample detection amount is large, the advantage that efficiency is high.
Embodiment
The invention provides one and grow tobacco and the assay method of tobacco product PetroChina Company Limited. ether extract total amount, comprising: A) be m by quality
0tobacco or tobacco product mix with sherwood oil, extract by accelerated solvent extraction, be extracted liquid; B) described extract is removed to desolventizing by decompression distillation, obtain the ligroin extraction that quality is m; Calculate tobacco or tobacco product PetroChina Company Limited. ether extract total amount; The massfraction that is tobacco or tobacco product PetroChina Company Limited. ether extract total amount is m/m
0.
Wherein, the present invention does not have special restriction to the source of all raw materials, for commercially available.
Be m by quality
0tobacco or tobacco product mix with sherwood oil, extract by accelerated solvent extraction.Wherein, described tobacco or tobacco product are preferably prepared according to standard YC/T31-1996; In described extraction, preferably also add drying agent, for preventing that at extraction process micro-water is dissolved in sherwood oil; Described drying agent is drying agent well known to those skilled in the art, there is no special restriction, is preferably anhydrous magnesium sulfate in the present invention; The pressure of described extraction is preferably 5～15MPa, more preferably 10～15MPa; The temperature of extraction is preferably 50 ℃～75 ℃, more preferably 60 ℃～75 ℃; The method of described extraction is method well known to those skilled in the art, there is no special restriction, preferably adopts static extracting in the present invention, and the time of extraction is preferably 3～10min, more preferably 5～8min; The number of times of extraction is preferably 3～5 times.
After extraction finishes, preferably rinse the abstraction pool of accelerated solvent extraction with sherwood oil, and with nitrogen blowing, preferably purge 80～200s, more preferably 80～100s; The volume that rinses sherwood oil used be preferably accelerated solvent extraction abstraction pool volume 50%～70%, more preferably 60%.Sherwood oil after flushing and extract merge.
Described extract is removed to desolventizing by decompression distillation, obtain the ligroin extraction that quality is m.The temperature of described decompression distillation is preferably 30 ℃～40 ℃; The solvent preferably distilling with collection with condensate water condensation when decompression distillation; The temperature of described condensate water is preferably-10 ℃～0 ℃; It is 2～3/s that the speed of described condensation is preferably controlled.
Be m/m by the above-mentioned massfraction that obtains tobacco or tobacco product PetroChina Company Limited. ether extract total amount
0.
The present invention also provides the assay method of another kind of tobacco and tobacco product PetroChina Company Limited. ether extract total amount, comprising: A ') be m by quality
0tobacco or tobacco product mix with sherwood oil, extract by accelerated solvent extraction, be extracted liquid; B ') described extract is removed to desolventizing by decompression distillation, obtain the ligroin extraction that quality is m; C ') sherwood oil is removed to desolventizing by decompression distillation, the extract quality obtaining in sherwood oil is m '; The quality of described sherwood oil and steps A ') in sherwood oil used identical in quality; The massfraction that calculates tobacco or tobacco product PetroChina Company Limited. ether extract total amount is (m-m ')/m
0.
Wherein, described extraction, decompression distillation are same as above, do not repeat them here.
Step C ') be blank test, in order to reduce the rear residual solids of sherwood oil volatilization to the impact of measuring.By steps A ') in the sherwood oil of equal quality remove desolventizing by decompression distillation, the extract quality obtaining in sherwood oil is m '; The massfraction of tobacco or tobacco product PetroChina Company Limited. ether extract total amount is (m-m ')/m
0.
In order further to improve the accuracy of tobacco and the total quantitative determination of tobacco product PetroChina Company Limited. ether extract, the present invention also provides one to grow tobacco and the assay method of tobacco product PetroChina Company Limited. ether extract total amount, comprising: A 〞) massfraction of measuring moisture in tobacco or tobacco product is ω H
2o; B 〞) be m by quality
0tobacco or tobacco product mix with sherwood oil, extract by accelerated solvent extraction, be extracted liquid; C 〞) described extract is removed to desolventizing by decompression distillation, obtain the ligroin extraction that quality is m; D 〞) sherwood oil is removed to desolventizing by decompression distillation, the extract quality obtaining in sherwood oil is m '; The quality of described sherwood oil and step B 〞) in sherwood oil used identical in quality; The massfraction that calculates tobacco or tobacco product PetroChina Company Limited. ether extract total amount is (m-m ')/m
0(1-ω H
2o).
Wherein, described extraction, decompression distillation are same as above, do not repeat them here.
In described tobacco or tobacco product, the assay method of moisture is method well known to those skilled in the art, there is no special restriction, is preferably the massfraction of measuring moisture in tobacco or tobacco product according to standard YC/T31-1996 in the present invention.
Now, the massfraction of tobacco or tobacco product PetroChina Company Limited. ether extract total amount is (m-m ')/m
0(1-ω H
2o).
For improving the accuracy of assay method, the present invention preferably carries out parallel experiment, and take the arithmetic mean value of twice replicate determination as measurement result, the absolute difference that is accurate to 0.1%, twice replicate determination should be not more than the arithmetic mean value of twice measured value.
The present invention utilizes accelerated solvent to extract and combines with reduced pressure distillation technique, measures the total amount of tobacco and tobacco product PetroChina Company Limited. ether extract, has the sample preparation time short, and sample detection amount is large, the advantage that efficiency is high.
In order to further illustrate the present invention, grow tobacco to provided by the invention one below in conjunction with embodiment and the assay method of tobacco product PetroChina Company Limited. ether extract total amount is described in detail.
In following examples, reagent used is commercially available.
Embodiment 1～3
Prepare tobacco leaf A1, A2 and the each 200g of A3 of three kinds of different year, different parts, three kinds of tobacco leaves are respectively divided into two parts of total amounts of measuring respectively tobacco leaf PetroChina Company Limited. ether extract by industry standard soxhlet extraction and following method.
Three kinds of tobacco leaf A1, A2 and A3 prepared to tobacco sample and measure moisture content according to standard YC/T31-1996, obtain powdered sample A1, A2 and the A3 of three kinds of tobacco leaves, recording three kinds of moisture in sample simultaneously and be respectively 12.51%, 13.02% and 12.88%.
Take respectively the each 5g(of tobacco Sample A 1, A2 and A3 and be accurate to 0.001g), per sample (p.s.) takes twice as parallel experiment, and the weight of sample is as shown in table 1; The sample taking is moved in the 10ml abstraction pool of accelerated solvent extraction, in abstraction pool, add 3g anhydrous sodium sulfate, for preventing that at extraction process micro-water is dissolved in sherwood oil, then in abstraction pool, add sherwood oil, with sherwood oil as extractant, at 10.34MPa(1500psi) under pressure, 70 ℃ of conditions, heating 5min, static extracting 5min, circulate 3 times, collect solution, with the sherwood oil flushing abstraction pool of abstraction pool volume 60%, and use nitrogen blowing 100s, the solution of the sherwood oil of flushing and collection is merged and is extracted liquid.
The 250ml heart bottle being placed in exsiccator is taken out, and weigh, obtain quality m
1; Extract is transferred to from receiving flask in 250ml heart bottle, and rinses and wash receiving flask with 5ml sherwood oil, rinse and wash three times, rinse washing lotion and be all transferred in heart bottle, 30 ℃ of deionization water-bath decompression condensation distillations, condensate temperature is-10 ℃, the control of solvent condenses speed is 2～3/s, until solvent frozen-free takes off heart bottle, clean outside with deionized water, dry with nonwoven fabrics again, be positioned over cool drying 0.5h in exsiccator, take out, take quality m
2(being accurate to 0.1mg).
Do blank test: in exsiccator, 250ml heart bottle is taken out, and weigh, obtain quality m simultaneously
3, and add and the blank sherwood oil of the suitable volume of extract, and decompression condensation distillation, until solvent frozen-free takes off heart bottle, clean outsidely with deionized water, then dry with nonwoven fabrics, be positioned over cool drying 0.5h in exsiccator, take out, take quality m
4(being accurate to 0.1mg).
The massfraction of tobacco sample PetroChina Company Limited. ether extract calculates by following formula, and what obtain the results are shown in Table 2:
Table 1 embodiment 1～3 takes the quality of tobacco test
Table 2 embodiment 1～3 tobacco sample PetroChina Company Limited. ether extract quality test results
Comparative example 1～3
Powdered sample A1, the A2 of three kinds of tobacco leaves of preparation in embodiment 1～3 and A3 are carried out to the mensuration of sample PetroChina Company Limited. ether extract content according to industry standard method.
Take respectively the each 2 ± 0.001g of tobacco Sample A 1, A2 and A3 in filtration paper cylinder, the weight of sample is as shown in table 3, clogs gently with absorbent cotton, puts into thermostatic drying chamber, in 80 ± 1 ℃ of dry 2h, and then before extracting, weighs the quality m of receiving bottle
1absorption bottle m with blank test
3filtration paper cylinder is put into extraction tube, filtration paper cylinder should be higher than the siphonal height of apparatus,Soxhlet's, filter paper packet length should be to be all soaked in sherwood oil and to be as the criterion, and adds 2/3rds places of sherwood oil reagent to receiving bottle volume in receiving bottle, connects extraction apparatus, connect condensate water, in the water-bath of 75 ± 1 ℃, heat, controlling sherwood oil reflow's cycle is 6～10 times per hour, and return time is 6h.
Extract completely, filtration paper cylinder is removed, still reclaim sherwood oil with former extraction tube, until steam stops volatilizing in receiving bottle, ligroin extraction is just stayed in receiving bottle; Receiving bottle is taken off, clean outsidely, the thermostatic drying chamber that is placed in 80 ± 1 ℃ is dried 2h, then in exsiccator cooling 0.5h, take quality m
2absorption bottle quality m with blank test
4; Dry again 0.5h, cooling equally, take quality, till being less than 0.001g to the difference of two inferior qualities.The massfraction of tobacco sample PetroChina Company Limited. ether extract calculates by following formula, and what obtain the results are shown in Table 4:
Table 3 comparative example 1～3 takes the quality of tobacco test
Table 4 comparative example 1～3 tobacco sample PetroChina Company Limited. ether extract quality test results
By the test of embodiment and comparative example, result shows, two kinds of methods, in the mensuration of ligroin extraction total amount, differ 0.1% and 0.2%, and difference is less than the experimental error of every kind of method 10%, and the numerical value that employing the inventive method records is within error range.
The above is only the preferred embodiment of the present invention; it should be pointed out that for those skilled in the art, under the premise without departing from the principles of the invention; can also make some improvements and modifications, these improvements and modifications also should be considered as protection scope of the present invention.
Claims (6)
1. one grow tobacco and the assay method of tobacco product PetroChina Company Limited. ether extract total amount, it is characterized in that, comprising:
A) be m by quality
0tobacco or tobacco product mix with sherwood oil, extract by accelerated solvent extraction, be extracted liquid;
B) described extract is removed to desolventizing by decompression distillation, obtain the ligroin extraction that quality is m;
Calculate tobacco or tobacco product PetroChina Company Limited. ether extract total amount.
2. one grow tobacco and the assay method of tobacco product PetroChina Company Limited. ether extract total amount, it is characterized in that, comprising:
A ') be m by quality
0tobacco or tobacco product mix with sherwood oil, extract by accelerated solvent extraction, be extracted liquid;
B ') described extract is removed to desolventizing by decompression distillation, obtain the ligroin extraction that quality is m;
C ') sherwood oil is removed to desolventizing by decompression distillation, the extract quality obtaining in sherwood oil is m '; The quality of described sherwood oil and steps A ') in sherwood oil used identical in quality;
Calculate tobacco or tobacco product PetroChina Company Limited. ether extract total amount.
3. one grow tobacco and the assay method of tobacco product PetroChina Company Limited. ether extract total amount, it is characterized in that, comprising:
A 〞) massfraction of measuring moisture in tobacco or tobacco product is ω H
2o;
B 〞) be m by quality
0tobacco or tobacco product mix with sherwood oil, extract by accelerated solvent extraction, be extracted liquid;
C 〞) described extract is removed to desolventizing by decompression distillation, obtain the ligroin extraction that quality is m;
D 〞) by step B 〞) in the sherwood oil of equal quality remove desolventizing by decompression distillation, the extract quality obtaining in sherwood oil is m '; The quality of described sherwood oil and step B 〞) in sherwood oil used identical in quality;
Calculate tobacco or tobacco product PetroChina Company Limited. ether extract total amount.
4. according to the assay method described in claim 1,2 or 3, it is characterized in that, described extraction also adds drying agent.
5. according to the assay method described in claim 1,2 or 3, it is characterized in that, the pressure of described extraction is 5～15MPa; The temperature of extraction is 50 ℃～75 ℃.
6. according to the assay method described in claim 1,2 or 3, it is characterized in that, the temperature of described decompression distillation is 30 ℃～40 ℃.
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Cited By (1)
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| CN106324145A (en) * | 2016-09-30 | 2017-01-11 | 中国烟草总公司郑州烟草研究院 | Distinguishing method of quality of fresh tobacco leaf sample in tobacco metabonomics based on terpenes |
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| CN104020073A (en) * | 2014-05-30 | 2014-09-03 | 江苏中烟工业有限责任公司 | Method of detecting the total amount of petroleum ether extracts in tobacco and tobacco products |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106324145A (en) * | 2016-09-30 | 2017-01-11 | 中国烟草总公司郑州烟草研究院 | Distinguishing method of quality of fresh tobacco leaf sample in tobacco metabonomics based on terpenes |
| CN106324145B (en) * | 2016-09-30 | 2018-06-15 | 中国烟草总公司郑州烟草研究院 | The method of discrimination of fresh tobacco leaves sample quality in a kind of tobacco metabolism group based on terpene |
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Application publication date: 20140625 |