CN102004132B - Method for measuring alkaloid in tobacco and tobacco product - Google Patents
Method for measuring alkaloid in tobacco and tobacco product Download PDFInfo
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Abstract
The invention relates to a method for measuring alkaloid in tobacco and tobacco products, which is characterized by dissociating alkaloid from the tobacco and tobacco products by using sodium hydroxide solution, extracting the alkaloid from samples by using triethylamine/trichloromethane solution, and detecting content of five kinds of alkaloid with GC-MS ( Gas Chromatograph-Mass Spectrum) quantitative analysis. Compared with other methods for analyzing the alkaloid, the invention has the advantages that alkaloid is separated from the tobacco by DB-35MS chromatographic columns so as to separate nornicotine and myosmine in the tobacco and accurately quantify target matters; batch sampling is carried out on the separation of nicotinamide and other alkaloid so as to detect the nicotinamide with high content in the tobacco and meet the quantitative analysis of other alkaloid with low content; the standard working curves of standard matters are separately compounded so as to avoid influence on quantization of other alkaloid by alkaloid catabolite existing in the standard samples. The method is simple and convenient and has the advantages of good repeatability, high analyzing and measuring sensitivity, and accurate quantization.
Description
Technical field
The invention belongs to the assay method of tobacco components, be specifically one grow tobacco and tobacco product in alkaloidal assay method.
Background technology
Alkaloid is the important component that influences quality of tobacco, and except that nicotine, alkaloid main in the tobacco also comprises nornicotine, anabasine, myosmine and anabasine.Nicotine can directly stimulate human central nervous, produces physiological reaction; Nornicotine has negative effect to cigarette odor-absorbing; Myosmine has a kind of mouse smell, has a strong impact on the suction flavor of cigarette product; The toxicity of anabasine is lower than nicotine slightly.Alkaloid is one of direct precursor of tobacco-specific nitrosamine; Burn and suck in the process easy metabolism for falling alkaloid at tobacco modulation and cigarette; And then the tobacco-specific nitrosamine, the especially nicotine that are formed with carcinogenicity with nitrite to transform to nornicotine be to cause one of principal element that tobacco leaf NNN and total TSNA content increases.U.S.'s tobacco industry was formulated nornicotine in the burley tobaccos tobacco leaf, anabasine and three kinds of the highest alkaloidal limiting the quantity of of anabasine in 1977; The ratio that these three kinds of alkaloid summations account for TA can not surpass 20%; Standard has been dropped to 15% in recent years; Other tobacco leaf major country of production men have also all formulated the nornicotine control criterion that individual plant is selected in tobacco leaf and the breed breeding, have fine qualities and higher availability to guarantee tobacco leaf.Therefore, alkaloid has important directive significance with the inherent quality of forming the understanding tobacco with the availability that improves tobacco leaf in the research tobacco.
At present China do not have also that a cover is complete, main secondary alkaloidal assay method in the tobacco of system, set up that main secondary alkaloidal assay method is very important in strong, reliable and stable tobacco of a cover applicability and the tobacco product.
Literature survey shows that the extraction of tobacco main alkaloid can be adopted soxhlet extraction, supersonic oscillations, SPME method.The soxhlet extraction time is longer, and the quantitative repeatability of SPME is relatively poor, and the extraction time of supersonic oscillations is short, and sample extraction is more complete, can be used as the best extracting process of tobacco main alkaloid.
The quantitative test great majority of tobacco main alkaloid adopt GC-FID, GC-NPD, GC/MS; The document of using HPLC separation determination nicotiana alkaloids is less; The method of capillary electrophoresis analysis also has report; But the capillary electrophoresis analysis instrument is very expensive, and the UV detecting device of employing is lower to some alkaloidal sensitivity, is not desirable analysis means.GC-FID is poor than GC-NPD to the selectivity that nitrogen-containing compound detects; And during the GC-NPD secondary alkaloid that content is lower in the detection by quantitative tobacco; Its sensitivity will be lower than GC/MS-SIM, so GC/MS-SIM is the first-selected analysis means of quantitative test nicotiana alkaloids.Literature survey in the past shows that there are three problems in the analysis of tobacco main alkaloid: 1) nicotine and other alkaloids content differ greatly in the tobacco, and the content of nicotine is tens milligrams of every grams normally; Like myosmine but is the every every grams of tens micrograms that restrain of several micrograms; When nicotine and myosmine were detected simultaneously, sample size was too small, and is bigger to the detection influence of myosmine; Sample size is excessive, and the detection limit of nicotine surpasses the respective range of detecting device again; 2) can not preferably nornicotine in the tobacco and myosmine be separated, what document usually adopted is the capillary column of DB-5ms because the hangover of the peak of nornicotine, influence with it go out the very near myosmine in peak separating with quantitatively; 3) nicotiana alkaloids quantitatively in, defective appears in the solution allocation of graticule curve.Because nicotine is prone to change into compounds such as nornicotine, myosmine, anabasine; Nornicotine also is prone to change into myosmine; So in the configuration of alkaloid graticule curve; Should be with the nicotine of being analyzed, nornicotine and other alkaloidal standard solution separate configuration, if mixed configuration will influence nornicotine and other is alkaloidal accurately quantitatively, but the solution allocation of graticule curve all is to adopt the configuration of standard specimen mixed solution in the document.Therefore, be necessary to develop a kind of easy and simple to handle, favorable reproducibility, sensitivity for analysis high, be fit to accurately quantitatively alkaloidal method in the tobacco.
Summary of the invention
The present invention is directed to the deficiency that exists in the existing analytical technology improves; Specialized designs nicotine and other alkaloidal method in a kind of while assay determination tobacco and the tobacco product; Utilize this method simple and convenient; Favorable reproducibility, assay determination is highly sensitive, can be accurately quantitative to nicotine in the tobacco and secondary alkaloid.
The objective of the invention is to realize: alkaloidal assay method in tobacco of the present invention and the tobacco product through following technical scheme; Utilize sodium hydroxide solution that the alkaloid in tobacco or the tobacco product is dissociated out; Employing contains the alkaloid in interior target triethylamine/chloroform soln extraction sample; Detect wherein nicotine, nornicotine, anabasine, myosmine and 5 kinds of alkaloids of anabasine through gas chromatography-mass spectrum (GC-MS) quantitative test, adopt internal standard method to carry out quantitative test.
Concrete steps are following:
(1) alkaloidal free in tobacco and the tobacco product: as to take by weighing 0.3g tobacco or tobacco product powder in 50mL triangular pyramidal bottle; The sodium hydroxide solution that adds 2.0mL mass percent 5% is in the triangular pyramidal bottle; The jog extraction flask, moistening sample leaves standstill and is no more than 25min;
(2) alkaloidal extraction and analysis in tobacco and the tobacco product: after nicotiana alkaloids is free; Add 20.0mL then and contain the triethylamine/chloroform extraction solution of internal standard compound matter; Seal and be placed in the supersonic wave cleaning machine; Ultrasonic Extraction, the ultrasonic Extraction time is 15min, ultrasonic power is 40Hz.Hold over night makes sample separate with extraction solution, gets 2mL lower floor solution after anhydrous sodium sulfate filters, and transfers to and treats the analysis of gas chromatography-mass spectrum sample introduction in the stratographic analysis bottle;
The gas chromatography-mass spectrometry analysis condition:
Chromatographic column: DB-35MS capillary column, long 30 m, internal diameter 0.25mm, thickness 0.25 μ m; Carrier gas: helium, flow rate of carrier gas: 1.0 mL/min; Injector temperature: 250 ℃; The detection of nicotine: sample size 1 μ l, split sampling, split ratio 40:1; The detection of nornicotine, myosmine, anabasine and anabasine: sample size 2 μ l, split sampling, split ratio 10:1;
Temperature programme: initial temperature: 100 ℃ keep 3min, rise to 260 ℃ with 8 ℃/min speed by 100 ℃, keep 10min, total run time 33min;
Detecting device: mass detector; Solvent delay: 8min; Ionization voltage: 70ev; Ion source temperature: 230 ℃; Transmission line temperature: 280 ℃; Scan ion scope: 33～400amu; Scanning of the mass spectrum mode: select ion monitoring (SIM).
The blending ratio of the used extraction solution triethylamine/methenyl choloride of the present invention is volume ratio 1: 10000.
It is 2-methylquinoline and 2 that interior mark is selected two interior marking, 4 '-second bipyridine, and nicotine is interior mark with the 2-methylquinoline, and other alkaloid is with 2, and 4 '-second bipyridine is interior mark; The concentration of 2-methylquinoline in extraction solution is 0.18mg/mL, 2, and the concentration of 4 '-second bipyridine in extraction solution is 10 μ g/mL.
During quantitative test; The configuration of the standard working curve of standard substance is carried out according to following method; Prepare the series standard working curve solution of nicotine separately; Prepare the series standard working curve solution of nornicotine separately, the series standard working curve solution of mixed preparing Mai Siming, anabasine and anabasine.
The advantage that the present invention compares prior art is: this method mainly is to utilize sodium hydroxide solution that the alkaloid in tobacco or the tobacco product is dissociated out; Adopt the alkaloid in 0.01% triethylamine/chloroform soln extraction sample, detect wherein 5 kinds of alkaloids content through gas chromatography-mass spectrum/selection ion monitoring (GC-MS/SIM) quantitative test.Analyze alkaloidal method with other and compare, the advantage of this method is, adopts DB-35MS chromatographic column separate tobacco alkaloid, can the nornicotine in the tobacco and myosmine be separated preferably, realizes accurately quantitative to object; The alkaloidal detection of nicotine and other is separated sample introduction, both can detect the higher nicotine of content in the tobacco, also can satisfy quantitative test the lower other biological alkali of content; The standard working curve of standard substance is preparation separately, has avoided the alkaloid catabolite influence quantitative to other alkaloid that exists in the standard specimen.This method extraction time is short, and is simple and convenient, favorable reproducibility, and the recovery is higher, and assay determination is highly sensitive, quantitatively accurately, is applicable to the analysis of batch samples.
Embodiment
The present invention further describes through following instantiation, but does not limit the present invention.
The assay instance:
Take by weighing 300mg tobacco or tobacco product powder in 50mL triangular pyramidal bottle, the sodium hydroxide solution that adds 2.0mL 5% in the triangular pyramidal bottle, the jog extraction flask, moistening sample leaves standstill and is no more than 25min.Add 20mL then and contain the triethylamine/chloroform extraction solution (the volume mixture ratio of triethylamine and methenyl choloride is 1:10000) in the triangular pyramidal bottle of internal standard compound matter; Seal and be placed in the supersonic wave cleaning machine; Ultrasonic extracting 15min, ultrasonic power are 40Hz, leave standstill then to make sample separate (placing 24h at most) with extractant; Get 2mL lower floor solution with anhydrous sodium sulfate dehydration after, transfer to and treat the analysis of gas chromatography-mass spectrum sample introduction in the stratographic analysis bottle.In mark select two in mark is 2-methylquinoline and 2,4 '-second bipyridine is interior mark, the quantitative employing 2-methylquinoline of nicotine is as interior mark, other alkaloidal quantitative employing 2,4 '-second bipyridine is as interior mark.
Adopt this method that 18 tobaccos and tobacco product are measured, wherein the flue-cured tobacco sample is 4,4 in burley tobaccos sample, 2 in Turkish tobaccos sample, 4 in Virginian-type cigarette pipe tobacco, 4 in blended type cigarette pipe tobacco.Measure the result and see table 1.
Table 1 tobacco sample alkaloid is measured result (μ g/g)
| Tobacco sample | Nicotine | Nornicotine | Myosmine | Anabasine | Anabasine |
| Flue-cured tobacco 1# | 24008.8 | 544.3 | 9.0 | 95.7 | 1924.6 |
| Flue-cured tobacco 2# | 16386.9 | 507.4 | 9.4 | 80.2 | 1998.9 |
| Flue-cured tobacco 3# | 20569.1 | 628.3 | 16.7 | 78.3 | 1431.8 |
| Flue-cured tobacco 4# | 21063.8 | 898.7 | 13.6 | 150.6 | 2297.4 |
| Burley tobaccos 1# | 63567.5 | 9885.7 | 188.0 | 346.0 | 8510.4 |
| Burley tobaccos 2# | 53090.8 | 5905.2 | 162.5 | 286.8 | 5766.0 |
| Burley tobaccos 3# | 41634.4 | 6073.0 | 118.7 | 319.3 | 4095.3 |
| Burley tobaccos 4# | 42647.3 | 2588.3 | 72.9 | 185.8 | 3874.7 |
| Turkish tobaccos 1# | 5453.4 | 257.6 | 9.7 | 17.3 | 177.1 |
| Turkish tobaccos 2# | 16146.5 | 538.7 | 18.3 | 41.4 | 677.3 |
| Virginian-type cigarette pipe tobacco 1# | 22794.1 | 745.8 | 11.8 | 133.0 | 2045.3 |
| Virginian-type cigarette pipe tobacco 2# | 23108.7 | 706.3 | 8.8 | 127.9 | 2099.6 |
| Virginian-type cigarette pipe tobacco 3# | 23636.2 | 639.0 | 9.5 | 121.7 | 1898.4 |
| Virginian-type cigarette pipe tobacco 4# | 22298.3 | 687.3 | 10.7 | 122.1 | 1870.7 |
| Blended type cigarette pipe tobacco 1# | 21375.0 | 1366.0 | 28.2 | 106.5 | 1799.8 |
| Blended type cigarette pipe tobacco 2# | 21946.1 | 1872.2 | 48.0 | 127.7 | 1985.0 |
| Blended type cigarette pipe tobacco 3# | 25203.9 | 2266.3 | 40.3 | 150.7 | 2487.6 |
| Blended type cigarette pipe tobacco 4# | 23781.5 | 1991.6 | 36.7 | 139.0 | 2209.9 |
The mensuration of working curve and detectability:
The mixing standard specimen of 6 variable concentrations is carried out the GC-MS analysis respectively; And carry out regretional analysis with the area ratio of the area of all types of target compound quota ion chromatographic peak and interior mark compound quota ion chromatographic peak and compound concentration and interior mark concentration ratio, obtain regression equation and correlation parameter thereof.With the standard solution replicate determination of least concentration 5 times, gained is measured 3 times of detectabilities (table 2) that are assay method of result standard deviation.The result shows that in the content range of main alkaloid, the mass detector response is good linear relationship with 5 kinds of compound concentrations in tobacco.
The range of linearity of table 2 analytical approach and detectability
| Compound | Concentration range (μ g/mL) | Regression equation | R 2 | Detectability (μ g/g) | Quantitative limit (μ g/g) |
| Nicotine | 30.43-1521.60 | y = 0.5115x - 0.0064 | 0.9996 | 14.1 | 46.8 |
| Nornicotine | 1.16-58.40 | y = 0.488x - 0.088 | 0.9992 | 2.3 | 7.6 |
| Myosmine | 0.028-1.392 | y = 0.2621x - 0.0005 | 0.9990 | 0.2 | 0.5 |
| Anabasine | 1.28-64.00 | y = 0.3614x - 0.0468 | 0.9991 | 1.5 | 5.1 |
| Anabasine | 0.8-40.00 | y = 0.1114x - 0.0132 | 0.9992 | 2.4 | 7.9 |
Repeatability, relative standard deviation and determination of recovery rates:
Same tobacco sample is carried out 5 times in a few days and replicate determination in the daytime (table 3-4), investigated the repeatability of method, a certain amount of standard specimen is added in the tobacco sample, carry out pre-treatment and quantitative test with the mark-on sample is parallel with mark-on sample not.And on high, medium and low three contents levels, carried out the mensuration (sample mark-on method, table 5) of the recovery.The result show the coefficient of variation that 5 kinds of VOCs measure the result in a few days, in the daytime respectively between 1.1%-3.9%, 1.7%-5.8%; The result of average recovery rate is between 91.1%～103.6%; Therefore this method repeatability is better, and the recovery is higher.The mensuration result of method is more accurate.
The mensuration of the repeatability in a few days result of table 3 method (μ g/g)
| Number of times | Nicotine | Nornicotine | Myosmine | Anabasine | Anabasine |
| 1 | 22675.5 | 491.1 | 6.5 | 105.5 | 1542.7 |
| 2 | 22966.8 | 499.4 | 6.4 | 106.3 | 1476.6 |
| 3 | 22266.5 | 496.8 | 6.5 | 101.5 | 1581.3 |
| 4 | 22622.7 | 509.9 | 6.8 | 111.6 | 1587.6 |
| 5 | 22513.3 | 526.0 | 6.3 | 111.0 | 1591.6 |
| Mean value | 22609.0 | 504.6 | 6.5 | 107.2 | 1555.9 |
| RSD（%） | 1.1 | 2.7 | 3.3 | 3.9 | 3.1 |
The mensuration of the repeatability in the daytime result of table 4 method (μ g/g)
| Fate | Nicotine | Nornicotine | Myosmine | Anabasine | Anabasine |
| The 1st day | 22598.9 | 509.4 | 6.8 | 111.5 | 1649.2 |
| The 2nd day | 23159.6 | 493.1 | 6.3 | 111.0 | 1591.6 |
| The 3rd day | 22967.2 | 515.1 | 6.2 | 103.9 | 1577.6 |
| The 4th day | 22559.8 | 458.0 | 7.1 | 116.7 | 1633.4 |
| The 5th day | 23488.9 | 536.4 | 6.6 | 102.9 | 1517.8 |
| Mean value | 22954.9 | 502.4 | 6.6 | 109.2 | 1593.9 |
| RSD（%） | 1.7 | 5.8 | 5.5 | 5.3 | 3.2 |
The recovery of table 5 method
| Alkaloid | Addition (μ g) | The recovery (%) | Addition (μ g) | The recovery (%) | Addition (μ g) | The recovery (%) | Average recovery rate (%) |
| Nicotine | 584.3 | 106.1 | 2921.6 | 104.3 | 14608.0 | 100.6 | 103.6 |
| Nornicotine | 11.7 | 90.2 | 29.2 | 93.9 | 146.0 | 101.6 | 95.2 |
| Myosmine | 0.3 | 88.8 | 0.7 | 96.5 | 3.5 | 99.5 | 94.9 |
| Anabasine | 12.8 | 91.8 | 32.0 | 97.1 | 160.0 | 101.8 | 96.9 |
| Anabasine | 8.0 | 87.2 | 20.0 | 91.0 | 100.0 | 95.2 | 91.1 |
The comparison of this method and tobacco business standard YC/T 246-2008
To the mensuration of nicotine, carried out the comparison test of this method and existing tobacco business standard YC/T246-2008 " the mensuration vapor-phase chromatography of tobacco and tobacco product nicotine " method, test figure is as shown in table 6.The result shows that the mensuration result's of two methods relative standard deviation explains that the mensuration result of two methods has good consistance in 4%, show that this method has reliable accuracy.
Table 6 tobacco sample nicotine measured value (mg/g)
| Tobacco sample | YC/T 246-2008 method | This method | Relative standard deviation (%) |
| Flue-cured tobacco | 23.1 | 21.8 | 4.0 |
| Burley tobaccos | 42.3 | 40.4 | 3.1 |
| Turkish tobaccos | 9.7 | 9.5 | 1.5 |
| Cigarette shreds | 18.8 | 17.9 | 3.7 |
Claims (4)
- One grow tobacco and tobacco product in alkaloidal assay method; It is characterized in that: utilize sodium hydroxide solution that the alkaloid in tobacco or the tobacco product is dissociated out; Employing contains the alkaloid in interior target triethylamine/chloroform soln extraction sample; Detect wherein nicotine, nornicotine, anabasine, myosmine and 5 kinds of alkaloids of anabasine through gas chromatography-mass spectrum (GC-MS) quantitative test, adopt internal standard method to carry out quantitative test, concrete steps are following:(1) alkaloidal free in tobacco and the tobacco product: as to take by weighing 0.3g tobacco or tobacco product powder in 50mL triangular pyramidal bottle; The sodium hydroxide solution that adds 2.0mL mass percent 5% is in the triangular pyramidal bottle; The jog extraction flask, moistening sample leaves standstill and is no more than 25min;(2) alkaloidal extraction and analysis in tobacco and the tobacco product: after nicotiana alkaloids is free; Adding 20.0mL contains the triethylamine/chloroform extraction solution of internal standard compound matter, and the blending ratio of triethylamine/chloroform extraction solution is volume ratio 1: 10000, seals to be placed in the supersonic wave cleaning machine; Ultrasonic Extraction; Hold over night makes sample separate with extraction solution, gets 2mL lower floor solution after anhydrous sodium sulfate filters, and transfers to and treats the analysis of gas chromatography-mass spectrum sample introduction in the stratographic analysis bottle;The gas chromatography-mass spectrometry analysis condition:Chromatographic column: DB-35MS capillary column, long 30 m, internal diameter 0.25mm, thickness 0.25 μ m; Carrier gas: helium, flow rate of carrier gas: 1.0 mL/min; Injector temperature: 250 ℃; The detection of nicotine: sample size 1 μ l, split sampling, split ratio 40:1; The detection of nornicotine, myosmine, anabasine and anabasine: sample size 2 μ l, split sampling, split ratio 10:1;Temperature programme: initial temperature: 100 ℃ keep 3min, rise to 260 ℃ with 8 ℃/min speed by 100 ℃, keep 10min, total run time 33min;Detecting device: mass detector; Solvent delay: 8min; Ionization voltage: 70ev; Ion source temperature: 230 ℃; Transmission line temperature: 280 ℃; Scan ion scope: 33～400amu; Scanning of the mass spectrum mode: select ion monitoring (SIM).
- 2. alkaloidal assay method in tobacco according to claim 1 and the tobacco product; It is characterized in that: it is 2-methylquinoline and 2 that interior mark is selected two interior marks, 4 '-second bipyridine, and nicotine is interior mark with the 2-methylquinoline; Other alkaloid is with 2, and 4 '-second bipyridine is interior mark; The concentration of 2-methylquinoline in extraction solution is 0.18mg/mL, 2, and the concentration of 4 '-second bipyridine in extraction solution is 10 μ g/mL.
- 3. alkaloidal assay method in tobacco according to claim 1 and the tobacco product is characterized in that: the ultrasonic Extraction time is 15min, and ultrasonic power is 40Hz.
- 4. alkaloidal assay method in tobacco according to claim 1 and the tobacco product; It is characterized in that: during quantitative test; The configuration of the standard working curve of standard substance is carried out according to following method; Prepare the series standard working curve solution of nicotine separately, prepare the series standard working curve solution of nornicotine separately, the series standard working curve solution of mixed preparing myosmine, anabasine and anabasine.
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