CN105158383B - A kind of method that ultrasonic wave added soxhlet extraction extracts Nicotiana tabacum L. oil - Google Patents
A kind of method that ultrasonic wave added soxhlet extraction extracts Nicotiana tabacum L. oil Download PDFInfo
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- CN105158383B CN105158383B CN201510399007.XA CN201510399007A CN105158383B CN 105158383 B CN105158383 B CN 105158383B CN 201510399007 A CN201510399007 A CN 201510399007A CN 105158383 B CN105158383 B CN 105158383B
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Abstract
The invention discloses a kind of method that ultrasonic wave added soxhlet extraction extracts oil in Nicotiana tabacum L., it comprises the steps：1）Weigh the Nicotiana tabacum L. of a certain amount of mesh number, load filter paper bag, be dried, cooling；2）By step 1）In filter paper bag put into the receiving bottle of Soxhlet extraction device, soak a period of time with a certain amount of petroleum ether；3）Ultrasonic method process step 2）In receiving bottle；4）Carry out surname extraction；5）Petroleum ether extract is concentrated；6）GC/MS tests and analyzes Nicotiana tabacum L. oil.The technique being proposed of the present invention and standard technique（YC/T176‑2003）Compare：Ligroin extraction total amount averagely improves more than 15%, and precision and repeatability are obvious, and solvent load is few, simple to operate.
Description
Technical field
The invention belongs to tobacco component extractive technique field, it is related to the extraction of oil in Nicotiana tabacum L., more particularly to a kind of super
Sound assists the method that soxhlet extraction extracts Nicotiana tabacum L. oil.
Background technology
Nicotiana tabacum L. is to plant widest industrial crops in the world, its chemical composition mainly include total sugar, total nitrogen, reducing sugar,
6 kinds of materials such as nicotine, potassium and chlorine.Nicotiana tabacum L. oil is the flavor matter that a class has Nicotiana tabacum L. characteristic perfume, is the reason of tobacco product
Think additive, its content height directly reflects the quality of quality of tobacco, improve oil content and can improve cigarette grade.Tobacco leaf oil
Point foot, on the one hand can keep " color, fragrant, taste, " of Medicated cigarette on the other hand can reduce the harm to health for the Nicotiana tabacum L..
Oil is a general concept, and its content is low, complicated component, mainly includes height according to pertinent literature report Nicotiana tabacum L. oil
Level fatty acid, Ester, western cypress trienes material and glucosides class etc., at present, do not have accurate boundary to the concept of Nicotiana tabacum L. oil
Fixed.The oil of therefore research Nicotiana tabacum L. has great importance it is necessary to carry out systematic study to it to improving cigarette quality.
Currently, the method extracting Nicotiana tabacum L. oil both at home and abroad mainly has steam distillation, Simultaneous distillation, Soxhlet to carry
Follow the example of, ultrasonic extraction etc..Ultrasonic extraction technology is a kind of new and high technology developed in recent years, soxhlet extraction with
Steam distillation compare with liquid-liquid extraction method with extraction efficiency high, solvent load is few, simple operation and other advantages.With ultrasonic method
Although the method extracting Nicotiana tabacum L. oil for pretreatment is common, DeGrain.
Content of the invention
Present invention aims to the defect of prior art, a kind of ultrasonic wave added soxhlet extraction is provided to extract Nicotiana tabacum L.
The method of middle oil, thus effectively improve the extracted amount of oil in Nicotiana tabacum L..
The purpose of the present invention is achieved through the following technical solutions.
（1）Weigh the Nicotiana tabacum L. of a certain amount of mesh number, load filter paper bag, be dried, cooling, weigh；
（2）By step（1）In filter paper bag put into the receiving bottle of Soxhlet extraction device, soak one with a certain amount of petroleum ether
The section time；
（3）Ultrasonic method process step（2）In receiving bottle；
（4）Filter paper bag in receiving bottle and petroleum ether are transferred in apparatus,Soxhlet'ses, receiving bottle adds 2 ~ 3 boilings
Stone and the petroleum ether of 148 ~ 152ml, reflux extraction certain time in 63 ~ 67 DEG C of water-baths；
（5）Take out filter paper bag, petroleum ether extract is concentrated, revolving is to 1ml at 44 ~ 46 DEG C；
（6）GC/MS tests and analyzes Nicotiana tabacum L. oil.
GC conditions are：
Chromatographic column：HP-5MS30m×0.25mm×0.25μm
Temperature programming：58 ~ 62 DEG C keep 290 ~ 310 seconds, rise to 133 ~ 137 DEG C with the speed of 4 DEG C/min；With 1 DEG C/min,
Rise to 173 ~ 177 DEG C；Again with 10 DEG C/min, rise to 308 ~ 312 DEG C, and keep 590 ~ 610 seconds；
Injector temperature：248 ~ 252 DEG C, sample size is 1 μ L；Carrier gas is high-purity He, flow rate of carrier gas 1ml/min；Solvent prolongs
6min late；Split ratio 10:1；
The present invention gives a kind of method that ultrasonic wave added soxhlet extraction extracts Nicotiana tabacum L. oil, and to sample therein at
Science and engineering skill conducts in-depth research, and to farthest extracting Nicotiana tabacum L. oil, improves yield；In the handling process of sample
Mainly consider six factors：Extraction time, ultrasonic power, ultrasonic time, soak time, granularity and solid-liquid ratio.
The impact to Nicotiana tabacum L. oil extraction ratio for the extraction time：Overall oil yield increases with the prolongation of extraction time
Reach maximum when greatly, between 6-8h, subsequently reduce and tend to balance.Analyzing its reason and may distilling is to carry out at ambient pressure, certain
A little unstable components may be aoxidized by the oxygen of in the air or pyrolysis directly occur；Carry out petrochina ether test
May volatilization loss a part, so that oil is also reduced.
The impact to Nicotiana tabacum L. oil extraction ratio for the ultrasonic power：Overall oil yield first increases with the increase extracting power
Maximum is reached, oil yield declines afterwards when greatly, between 70-75W.Analyze the increase with ultrasonic power for its reason, experiment
Condition becomes violent, increases the volatile quantity of petroleum ether, so that the low boiling component in oil is also lost with the volatilization of medium.
The impact to Nicotiana tabacum L. oil extraction ratio for the ultrasonic time：Overall oil yield first increases with the prolongation of ultrasonic time
Greatly, in 50min about reach maximum, the prolongation tobacco oil with ultrasonic time is got rate and is declined on the contrary afterwards.Analyze it former
Because being probably that with the prolongation of ultrasonic time, tobacco cell is constantly destroyed, and the oil in Nicotiana tabacum L. is not under certain ultrasonic power
Break and ooze out, so that reaching maximum；With the prolongation further of ultrasonic time, petroleum ether constantly volatilizees, and makes in Nicotiana tabacum L. oil
A low boiling component also volatilization loss part.
The impact to Nicotiana tabacum L. oil extraction ratio for the soak time：Overall oil yield first increases with the prolongation of soak time
Plus, in 12h about reach maximum, the prolongation of subsequent soak time, the yield of Nicotiana tabacum L. oil is not changed significantly.Analysis
Its reason is probably the prolongation with soak time, and Nicotiana tabacum L. is sufficiently soaked, and is further added by soak time, and oil extracts
Rate there will not be significant increase.
The impact to Nicotiana tabacum L. oil extraction ratio for the granularity：Overall Nicotiana tabacum L. oil extraction ratio first increases with the increase of granularity
Greatly, reach maximum about 40 mesh, reduce with the increase of granularity afterwards, finally tend to balance.Analyzing its reason is probably
The undue increase of granularity, makes volatile component in Nicotiana tabacum L. oil also constantly lose, is unfavorable for the extraction of oil.
The impact to tobacco leaf oil extraction ratio for the solid-liquid ratio：Solid-liquid ratio is 1:40-1:When between 80, with the increasing of solid-liquid ratio
Greatly, oil extraction ratio constantly increases, until maximum.Reason is probably：With the continuous increase of solid-liquid ratio, Nicotiana tabacum L. is made to be filled
The immersion dividing, thus reaching more preferable plasmolysis effect, is more beneficial for oozing out of Nicotiana tabacum L. oil；Solid-liquid ratio is 1:80-1:100
Between when, with the increase of solid-liquid ratio, oil extraction ratio has a declining tendency again.
Consider above six factors, maximum yield will be obtained, best treatment conditions are as follows：Extraction time 4h, surpasses
Acoustical power 70W, ultrasonic time 40min, soak time 12h, granularity 40 mesh, solid-liquid ratio 1:80.
The invention has the beneficial effects as follows：The present invention is studied to Nicotiana tabacum L. oil using ultrasonic wave added soxhlet extraction, with
National Standard Method（YC/T176-2003）Compare, oil extraction ratio improves more than 15%.The relative standard deviation of experimental result
（RSD/%）It is significantly less than National Standard Method it is seen that the precision of ultrasonic wave added soxhlet extraction and repeatability are substantially better than National Standard Method.This
Invention detects that β-terpinene, adjacent nicotine, nicotyrine, different Buddhist nun are ancient first in the petroleum ether extract that Nicotiana tabacum L. oil extracts
Fourth, trans Squalene, caryophyllin, 7 kinds of materials of (Z)-caryophyllene.In addition method solvent load of the present invention is few, operation letter
Single, it is worth exploring and study.
Specific embodiments
Embodiment 1
For further appreciate that the present invention, with reference to specific embodiment, above-mentioned technical scheme is done further
Illustrate and explanation.
The reagent used in following examples, the concrete condition of equipment are shown in Table 1, table 2.
Table 1 experiment reagent
| Title | Purity | Manufacturer |
| Dichloromethane | Analysis is pure（AR） | Tianjin Fengchuan Chemical Reagent Science ＆ Technology Co., Ltd. |
| Anhydrous sodium sulfate | Analysis is pure（AR） | Tianjin Yao Hua chemical reagent Co., Ltd |
| Sodium chloride | Analysis is pure（AR） | Tianjin Kermel Chemical Reagent Co., Ltd. |
Table 2 experimental facilitiess
| Title | Manufacturer |
| RE-2000B type rotary evaporator | Yuhua Instrument Co., Ltd., Gongyi City |
| SHZ-D (III) type circulating water type vacuum pump | Yu Hua Instrument Ltd. of Henan Province |
| FW-400A type tilting high speed Universal pulverizer | Beijing Zhong Xing great achievement Instrument Ltd. |
| Electronic analytical balance | Beijing Sai Duolisi instrument system company limited |
| DZKW-C type electronic thermostatic water-bath | Shanghai leap medical apparatus and instruments factory |
| Electric jacket | Yuhua Instrument Co., Ltd., Gongyi City |
| Unification of the motherland standard screen | Shangyu city of Zhejiang Province Shun Long experimental apparatus factory |
The method that concrete USEM method calculates the extraction ratio of Nicotiana tabacum L. oil：
1. the mensure of laboratory sample moisture content
In experiment, the mensure of tobacco sample moisture content adopts the Oven Method in Y C/T31- 1996, as follows：
1）Empty tared dish is put in baking oven,（100 scholars 1）Dry 2h at DEG C, cool down 30min in exsiccator, weigh and be
m0.
2）Add the cigarette sample of 1.998 ~ 2.002g in tared dish, be weighed as m1.
3）The tared dish putting into cigarette sample is put into baking oven,（100 scholars 1）Dry 2h at DEG C, in exsiccator, cool down 30min,
Weigh as m2.
The moisture content of sample is calculated as follows：
W=(m1—m2)/(m1—m0)*100% (3.1)
In formula：The moisture content of W sample, %；
m0Tared dish quality, g；
m1The gross mass of tared dish and sample, g before drying；
m2The gross mass of tared dish and sample, g after drying.
2. Nicotiana tabacum L. oil extraction step
1）Accurately weigh the tobacco sample of 1.998 ~ 2.002g40 mesh, load in filter paper bag, filter paper bag is put into weighing botle,
2 hs are dried at 80 DEG C.Take out, exsiccator cools down about 30 min, weigh.
2）Filter paper bag is put in the receiving bottle of Soxhlet extraction device, adds a certain amount of（The volume of petroleum ether did not just have
Filter paper bag, 148 ~ 152ml）Petroleum ether, with preservative film sealing, under room temperature soak 12h.
3）Ultrasonic device is modulated under the frequency of 45khz, by ultrasonic for receiving bottle 40min under the ultrasonic power of 70w.
4）Filter paper bag in receiving bottle and petroleum ether are transferred in apparatus,Soxhlet'ses, receiving bottle adds 2 ~ 3 boilings
Stone and the petroleum ether of 150ml, reflux extraction 4h in 65 DEG C of water-baths.
5）Take out filter paper bag, 80 DEG C in the baking oven at 2 hs are dried, exsiccator cools down about 30 min, weighs.To connect
Receive bottle in petroleum ether extraction liquid transfer in revolving bottle, at 45 DEG C revolving to 1ml, in case analysis use.
3. blank experiment step
1）Filter paper bag is put in weighing botle, 2 hs are dried at (80.0 ± 1) DEG C.Take out, cool down about in exsiccator
30min, weighs.
2）According to above-mentioned steps 2 and 3, filter paper bag is processed.
3）Take out filter paper bag, 2 hs are dried at (80.0 ± 1) DEG C in the baking oven, exsiccator cool down about 30 min, claims
Amount.
The extraction ratio of Nicotiana tabacum L. oil is calculated using weight reduction, and formula is as follows：
Tobacco oil gets rate/%=（M1-M2）-(M3-M4)/M0*(1-W)*100%
M0Actual weighing quality (g) of=tobacco sample
M1The quality of tobacco sample and filter paper bag before=experiment（g）
M2The quality of tobacco sample and filter paper bag after=experiment（g）
M3The quality of air filter paper bag before=experiment（g）
M4The quality of air filter paper bag after=test（g）
W=refers to the moisture content (%) in tobacco sample
Choose National primary standard flue-cured tobacco sample upper leaf, middle leaf, inferior leads totally three in 2013, respectively B3F, C3F,
X3F.Its Content of Petroleum Ether Extract is measured respectively using USEM method and standard technique, each sample parallel assay 7 times.Upper leaf
B3F sample ligroin extraction total amount, USEM method improves 24.141% than standard technique；Middle leaf C3F sample ligroin extraction
Total amount, USEM method improves 17.292% than standard technique；Inferior leads X3F sample ligroin extraction total amount, USEM method carries than standard technique
High 16.483% it is seen that USEM method averagely improves more than 15% than standard technique ligroin extraction total amount.
Embodiment 2
The concrete extraction step repeating Nicotiana tabacum L. oil in embodiment 1 is to table mountain C032, Nanping, Fujian C015, Luoyang Luoning
Tetra- kinds of different tobacco samples of C3F and Zambia ZM-BOAT are extracted, and carry out into go-on-go using GC/MS instrument to extract
Survey, four kinds of different sample detection compositions are analyzed.
GC/MS combination instrument and testing conditions
GC conditions are：
Chromatographic column：HP-5MS(30m×0.25mm×0.25μm)
Temperature programming：60 DEG C of holding 5min, rise to 135 DEG C with the speed of 4 DEG C/min；With 1 DEG C/min, rise to 175 DEG C；Again
With 10 DEG C/min, rise to 310 DEG C, and keep 10min.
Injector temperature：250 DEG C, sample size is 1 μ L；Carrier gas is high-purity He, flow rate of carrier gas 1ml/min；Solvent delay
6min；Split ratio 10:1
Mass Spectrometer Method condition：
EI ion source temperature：230℃；Ion source electron energy：60ev；Mass scan range is 35-500u.
Example 2 draws in the petroleum ether extract of Nicotiana tabacum L. oil and detects 97 kinds of materials altogether, according to the classification of chemical composition,
Including alkaloidss（5 kinds）, alcohols（13 kinds）, hydro carbons（26 kinds）, acids（6 kinds）, ketone（11 kinds）, aldehydes（4 kinds）, esters
（15 kinds）, phenols（4 kinds）, pyroles（1 kind）, pyridines（1 kind）, furans（1 kind）, miazines（1 kind）, amide-type（1 kind）、
Anhydrides（1 kind）, the fragrant same clan（7 kinds）Deng 14 kinds.And in Nicotiana tabacum L. oil, extraction and analysis go out β-terpinene, adjacent Buddhist nun's Gu first
Fourth, nicotyrine, isonicotine, trans Squalene, caryophyllin, 7 kinds of materials of (Z)-caryophyllene.Its analysis result is as shown in table 3.
The constituent of oil in table 3 Nicotiana tabacum L.
The constituent of oil in continued 3 Nicotiana tabacum L.
The constituent of oil in continued 3 Nicotiana tabacum L.
The constituent of oil in continued 3 Nicotiana tabacum L.
Claims (6)
1. a kind of method that ultrasonic wave added soxhlet extraction extracts Nicotiana tabacum L. oil, comprises the steps：
（1）Weigh the tobacco sample of a certain amount of mesh number, load filter paper bag, be dried, cooling, weigh；
（2）By step（1）In filter paper bag put into the receiving bottle of Soxhlet extraction device, when soaking one section with a certain amount of petroleum ether
Between；
（3）Ultrasonic method pre-treatment step（2）In receiving bottle；
（4）Filter paper bag in receiving bottle and petroleum ether are transferred in apparatus,Soxhlet'ses, receiving bottle adds a certain amount of boiling
Stone and the petroleum ether of 80 ~ 160ml, reflux extraction certain time in 64 ~ 66 DEG C of water-baths；
（5）Take out filter paper bag, petroleum ether extract is concentrated, revolving is to certain volume at 44 ~ 46 DEG C；
（6）GC/MS tests and analyzes Nicotiana tabacum L. oil；
GC conditions are：
Chromatographic column：HP-5MS30m×0.25mm×0.25μm；
Temperature programming：58 ~ 62 DEG C keep 290 ~ 310 seconds, rise to 133 ~ 137 DEG C with the speed of 4 DEG C/min；With 1 DEG C/min,
Rise to 173 ~ 177 DEG C；Again with 10 DEG C/min, rise to 308 ~ 312 DEG C, and keep 590 ~ 610 seconds；Injector temperature：248~
252 DEG C, sample size is 1 μ L；Carrier gas is high-purity He, flow rate of carrier gas 1ml/min；Solvent delay 6min；Split ratio 10:1 ；
Mass Spectrometer Method condition
EI ion source temperature：228~232℃ ；Ion source electron energy：60ev ；Mass scan range is 35-500u.
2. as described in claim 1 extraction Nicotiana tabacum L. oil method it is characterised in that：The granularity of tobacco sample is 40 mesh.
3. as described in claim 1 extraction Nicotiana tabacum L. oil method it is characterised in that：Petroleum ether soak time is 6 ~ 16h.
4. as described in claim 1 extraction Nicotiana tabacum L. oil method it is characterised in that：Ultrasonic power is 70W, ultrasonic time
30~60min.
5. as described in claim 1 extraction Nicotiana tabacum L. oil method it is characterised in that：Soxhlet extraction extraction time be 3 ~
9h.
6. as described in claim 1 extraction Nicotiana tabacum L. oil method it is characterised in that：Sample and the quality volume of extracting solution
Than：1:40~1:100.
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| CN105699561A (en) * | 2016-02-29 | 2016-06-22 | 中国烟草总公司广东省公司 | Method for detecting squalene in tobacco leaves |
| CN105628827A (en) * | 2016-02-29 | 2016-06-01 | 中国烟草总公司广东省公司 | Liquid sample preparation method for detecting squalene contained in cigarette smoke through high performance liquid chromatography method |
| CN105699553A (en) * | 2016-02-29 | 2016-06-22 | 中国烟草总公司广东省公司 | Sample pretreatment method for detection of squalene in cigarette smoke |
| CN107144660A (en) * | 2016-12-30 | 2017-09-08 | 中国烟草总公司广东省公司 | Perfumery is caused to build method and the application of tobacco leaf finger-print in a kind of surname extraction tobacco leaf by methanol |
| CN106701313A (en) * | 2017-03-07 | 2017-05-24 | 重庆科技学院 | Method for extracting hermetia illucens larva oil through ultrasound-assisted soxhlet extraction method |
| CN110591824A (en) * | 2019-10-17 | 2019-12-20 | 山西农业大学 | Extraction process of folium artemisiae argyi volatile oil |
| CN116429948A (en) * | 2023-05-11 | 2023-07-14 | 山东金胜粮油食品有限公司 | Method for rapidly extracting fatty acid composition from fat measurement in high-oleic-acid peanuts |
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| CN102559388A (en) * | 2012-02-27 | 2012-07-11 | 浙江中烟工业有限责任公司 | Essential oil of tobaccos as well as preparation method and application thereof to cigarettes |
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