CN102796076A - Preparation method for nicotine standard substance - Google Patents
Preparation method for nicotine standard substance Download PDFInfo
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- CN102796076A CN102796076A CN201210319785XA CN201210319785A CN102796076A CN 102796076 A CN102796076 A CN 102796076A CN 201210319785X A CN201210319785X A CN 201210319785XA CN 201210319785 A CN201210319785 A CN 201210319785A CN 102796076 A CN102796076 A CN 102796076A
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Abstract
The invention relates to a preparation method for a nicotine standard substance. The preparation method for the nicotine standard substance comprises the following steps: a, preparing coarse nicotine: adding ground waste tobacco into sodium hydroxide aqueous solution, stirring in water bath and extracting; filtering and adjusting the pH value of the filtrate by using sodium hydroxide to obtain nicotine extracting solution; distilling and concentrating the nicotine extracting solution, taking out the concentrated solution, cooling, adding sodium hydroxide aqueous solution and adjusting the pH value to be 11 to obtain the concentrated distillate; adding the concentrated distillate into chloroform, extracting and dehydrating the extracting solution by using anhydrous sodium sulfate to obtain the coarse nicotine solution; and b, preparing pure nicotine: performing reduced-pressure distillation and purification on the coarse nicotine obtained in the step a or the commercial coarse nicotine with the purity of not less than 60 percent under the conditions of pressure of 4.5-6.5 kPa and temperature of 160-170 DEG C to obtain pure nicotine; and subpackaging into a plurality of brown ampoule bottles of 1.0 mL under the protection of nitrogen and storing in a refrigerator at the temperature of 0 to 4 DEG C in dark place.
Description
Technical field
The present invention relates to a kind of reference material of nicotine, relate to a kind of preparation method of nicotine reference material specifically.
Background technology
(have another name called Nicotine, Nicotine), its chemical name is: 3-(1-methyl-2-pyrrolidyl) pyridine or 1-methyl-2-(2-pyridyl) pyrrole are pressed against alkane to nicotine.CAS 54-11-5.Structural formula is following:
Pure nicotine at room temperature is colourless or pale yellow oily liquid body, has left-handed photosensitiveness, and density is 1.0071 in the time of 20 ℃, and 247 ℃ of boiling points have strong sharp flavor, and deliquescence is arranged.Can generate hydrate with water in time below 60 ℃, be soluble in the organic solvents such as alcohol, ether, chloroform and sherwood oil, and can steam with water vapor.
The height of nicotine content is an important indicator of tobacco leaf and cigarette quality control in the tobacco, greatly influences the strength of cigarette smoking.Along with going deep into of the development of tobacco research and production, particularly smoking and health research, tobacco components analysis and research work has received very big attention.
At present, the cigarette national standard has had more strict regulation to the nicotine content in the cigarette smoke TPM, and this accuracy to determination data is had higher requirement.But through login international reference materials DB (International Data Bank on Certified Reference Materials COMAR) http://www.comar.bam.de/home/index.php and national standard material information platform http://www.ncrm.org.cn inquiry, various countries all do not have the registration of nicotine reference material at present.Each big tobacco enterprise mostly uses the nicotine reagent that U.S. SIGMA reagent company produces in the world, does not have the standard definite value yet its shortcoming is this nicotine reagent, and a content range only is provided.Therefore, development nicotine reference material is significant for the safety that guarantees the correlative study analytical data.
Summary of the invention
The object of the invention just is being based on above-mentioned prior art situation and the preparation method of a kind of nicotine reference material of developing.
The objective of the invention is to realize through following technical scheme:
The preparation method of nicotine reference material of the present invention may further comprise the steps:
The preparation method of a, thick nicotinic
At first, get inferior tobacco 1 kg after grinding, the aqueous sodium hydroxide solution that adds 4～5L, 0.1 mol/L carries out stirring in water bath and extracts, and extracts temperature at 50～60 ℃, stirs 4～6 hours extraction times; Filter then, filtrating is adjusted pH=11 with sodium hydroxide, and this solution is the nicotine extracting solution; Then, the nicotine extracting solution is distilled processing, 100～110 ℃ of distillation temperatures, when the distillate of collecting account for be distilled volume 60～70% the time, stop distillation, obtain distillate; Once more, will slip out liquid and concentrate, 100～110 ℃ of thickening temperatures, when the liquid concentrator volume be effluent volume 1/3 ~ 1/4 the time, take out liquid concentrator, add sodium hydroxide solution after cooling and regulate pH=11, obtain spissated distillate; At last, spissated distillate is added chloroform extract, extraction liquid is used anhydrous sodium sulfate dehydration, obtains thick nicotinic solution;
B, pure nicotine preparation method
The thick nicotinic that is obtained among the step a or purity are not less than 60% commercialization thick nicotinic, are that 4.5 ~ 6.5 kPa, temperature are that underpressure distillation is purified, and obtains pure nicotine under 160～170 ℃ the condition at pressure; Under adopting the condition of nitrogen protection, be loaded in the brown container of handling through sterilizing-drying, under the condition of lucifuge, leave in 0 ℃ ~ 4 ℃ the refrigerator and preserve.
Brown container described in the step b is made up of the brown ampoule of several 1.0 mL.In the present invention, used thick nicotinic generally is a nicotine extract of choosing inferior tobacco, also can require nicotine purity generally should not be lower than 60%, to guarantee certain nicotine extraction yield through buying commercial thick nicotinic.
In the present invention, used brown ampoule should pass through the sterilizing-drying processing; The nicotine reference material that is obtained has good uniformity, and this reference material is stable in 1 year, and the definite value result of the nicotine reference material that is obtained is 98.5%, and expanded uncertainty is 0.6 %.
Nicotine reference material of the present invention has good uniformity, and stable in 1 year probation, the control experiment result is good between the laboratory.The standard value of this reference material and uncertainty thereof are
, can guarantee carry out the traceability of measurement of correlation work.
In the present invention, the valued methods that is adopted is that International Standards Method ISO13276:1997 " the mensuration silicotungstic acid weighting method of tobacco and tobacco product nicotine purity " measures.This method is No. 39 recommend method of international tobacco scientific research cooperative association (CORESTA), and is converted into tobacco industry standard (YC/T 247-2008) in 2008, at home and abroad is widely used, and has good tolerance range (repeatability).
In the present invention, the valued methods of employing is to be accomplished by 6 tame laboratory cooperation definite values, and the approval of CNAL (CNAS) has all been passed through in the six tame laboratories of participating in definite value, has the essential condition of nicotine reference material definite value.
The nicotine reference material that utilizes the inventive method to develop; Can be used for chemical analysis, quality control and the check of tobacco and association area; Realize measuring the instrument of traceability as association area; Thereby under the prerequisite that guarantees the measuring result quality, simplify the program that realizes that analysis to measure is traced to the source greatly.
The present invention compared with prior art has following beneficial effect:
(1) the present invention has developed the reference material of nicotine first at home, and the standard value of this reference material and uncertainty thereof are
;
(2) the nicotine reference material of the present invention's development has good uniformity, and it is stable that the study on the stability result is illustrated in 1 year interior this reference material of probation;
(3) development of this nicotine reference material is expected in national tobacco industry quality inspection system and association area, promote, and has great application prospect.
Description of drawings
Fig. 1 nicotine reference material development technology.
Fig. 2 nicotine typical case TIC color atlas.
Fig. 3 nicotine mass spectrum and NIST spectrum storehouse corresponding diagram.
Embodiment
The present invention does below in conjunction with embodiment and further describes, but is not restriction the present invention.
The preparation method of nicotine reference material of the present invention may further comprise the steps:
A. the preparation method of thick nicotinic
At first, get inferior tobacco 1 kg after grinding, the aqueous sodium hydroxide solution that adds (4～5) L 0.1 mol/L carries out stirring in water bath and extracts, and extracts temperature in (50～60) ℃, stirs extraction time (4～6) hour.Filter then, filtrating is adjusted pH=11 with sodium hydroxide, and this solution is the nicotine extracting solution.Then, the nicotine extracting solution is distilled processing, distillation temperature (100～110) ℃ when the distillate of collecting accounts for (60～70) % that is distilled volume, stops distillation, obtains distillate.Once more, will slip out liquid and concentrate, thickening temperature (100～110) ℃, when the liquid concentrator volume be effluent volume 1/3 ~ 1/4 the time, take out liquid concentrator, add sodium hydroxide solution after cooling and regulate pH=11, obtain spissated distillate.At last, spissated distillate is added chloroform extract, extraction liquid is used anhydrous sodium sulfate dehydration, obtains thick nicotinic solution.
B. pure nicotine preparation method
With the thick nicotinic or the commercial thick nicotinic (purity is not less than 60%) that are obtained in the last step, be (4.5 ~ 6.5) kPa at pressure, temperature is that the underpressure distillation purification obtains pure nicotine under the condition of (160～170) ℃.Be sub-packed in nitrogen protection in the brown ampoule of 1.0 mL, outsourcing black kraft paper, 10 one boxes amount to 50 boxes, leave in 0 ℃ ~ 4 ℃ the refrigerator, keep in Dark Place.
C. uniformity testing
The nicotine reference material belongs to liquid pure article standard material.The general easy and uniform of liquid, the unit number that therefore extracts can be the lower limit of " primary standard material technical specifications " defined.This experiment is extracted 7 bottles, 6 bottles, 6 bottles samples respectively in initial, the centre and the termination stage of the packing of nicotine sample, and totally 19 bottles of samples carry out uniformity testing, every bottle of sample replication 3 times.Carry out uniformity testing between interior uniformity testing of bottle and bottle.The sampling amount of this measuring method is 100 mg.
Nicotine reference material uniformity testing take off data result such as table 1; Under significance level
, data are carried out statistical study in the employing F method of inspection his-and-hers watches 1.Can get by data in the table 1:
Annotate: S1---standard deviation between group;
S2---the group internal standard is poor;
Q1---variance between laboratories;
Q2---variance within laboratory;
F calculates---the F test statistic
F (ν 1, and ν 2)---the F-distribution statistic of degree of freedom (ν 1, and ν 2).
The pure nicotine reference material of table 1 uniformity testing take off data (%)
D. stability test evaluation
Nicotine reference material stability test take off data result such as table 2 with the time do
x, measuring result does
y, in significance level
Adopt method of least squares to return in the T method of inspection his-and-hers watches 2 data and carry out statistical study down.Data by table 2 can get:
Process statistics amount:
Straight-line equation slope:
The standard deviation of residual error:
The uncertainty relevant:
with slope
The pure nicotine reference material of table 2 STABILITY MONITORING take off data (%)
E. definite value
This project adopts six tame laboratory cooperation definite values, comparison and checking.Six tame laboratories are respectively national tobacco quality supervision and inspection center, tobacco quality supervision and inspection station, Guangdong Province, tobacco quality supervision and inspection station, Yunnan Province, tobacco quality supervision and inspection station, Shanghai City, tobacco quality supervision and inspection station, northwest and tobacco quality supervision and inspection station, Hubei.The approval of CNAL (CNAS) has all been passed through in this six tame laboratory, has the essential condition of nicotine reference material definite value, and has certain technology authoritative.
The statistical test of value data is confirmed the validity of take off data through F check and observed value normal distribution inspection, test of outlier between accuracy test, groups such as group intermittent gauging value, and the result sees table 3.Visible from The result of statistics, the take off data in the table 3 is valid data.Therefore, the population mean 98.5% of getting six laboratory measurement data MVs in the table 6 is as the definite value result, and this definite value is the standard value of nicotine reference material purity.
Table 3 nicotine purity definite value assay (%)
F. uncertainty evaluation
Through analyzing the uncertainty that each laboratory nicotine purity definite value result's uncertainty source has the sample ununiformity to cause
u R1The uncertainty that sample measurement repeatability produces
u R2The uncertainty u that balance measurement produces
R3The uncertainty u that permanent stability are introduced
R4
1) uncertainty that causes of sample ununiformity
u R1
Adopt table 1 data,
does by the caused standard deviation of material ununiformity
The standard deviation
that method is measured does
The result shows that the standard deviation size that standard deviation that ununiformity produced and method are measured is close, at this moment need the homogeneity factor be taken into account as the total uncertainty of reference material.Therefore, the relative uncertainty that is caused by the sample ununiformity is:
2) uncertainty of sample measurement repeatability generation
u R2
Through check, 6 tame laboratory raw data (like table 3) Normal Distribution, and 6 tame laboratories are respectively organized and precision such as are between the data.Therefore, 6 tame experimental determination results' MV is regarded as one group of new take off data, obtains with statistical method.Its relative standard uncertainty is
3) uncertainty of balance measurement generation
u R3
Through calibrating, when 0≤m≤50g, the error of balance weighing is 0.1 mg.In experimentation, take by weighing nicotine 1 time; Constant weight crucible 2 times (by difference), weighing are considered uniform distribution by 100 mg.Its relative standard uncertainty is
4) uncertainty of permanent stability introducing
u R4
Adopt different time (12 months) take off data in the table 2, with the time do
x, with
yRepresent the eigenwert of reference material, fitting a straight line is also calculated the uncertainty of closing earlier with slope, and validity period is according to calculating December (1 year).The relative uncertainty that its permanent stability are introduced
u r3
For
5) synthetic uncertainty
Combined standard uncertainty does
Expanded uncertainty
，
Get
,
The nicotine reference material of being developed among the present invention is identified through China National Measuring Science Research Inst.'s stoichiometry and analysis science institute; The purity of the nicotine reference material of this project preparation is 98.4%; The definite value result 98.5% of this and this reference material is very identical, explains that comparison is good with the checking result between the laboratory of this nicotine reference material.
With gas chromatograph-mass spectrometer this reference material is analyzed, the area normalization method quantitative Analysis, this reference material purity is 99.2%.Good with the similarity of the corresponding fragment ion in corresponding NIST spectrum storehouse through prepared nicotine reference material, purity is consistent with the definite value result.Typical case TIC color atlas, nicotine mass spectrum rod figure and the corresponding spectrogram of NIST are shown in Fig. 2～3.
Claims (3)
1. the preparation method of a nicotine reference material, it is characterized in that: it may further comprise the steps:
The preparation method of a, thick nicotinic
At first, get inferior tobacco 1 kg after grinding, the aqueous sodium hydroxide solution that adds 4～5L, 0.1 mol/L carries out stirring in water bath and extracts, and extracts temperature at 50～60 ℃, stirs 4～6 hours extraction times; Filter then, filtrating is adjusted pH=11 with sodium hydroxide, and this solution is the nicotine extracting solution; Then, the nicotine extracting solution is distilled processing, 100～110 ℃ of distillation temperatures, when the distillate of collecting account for be distilled volume 60～70% the time, stop distillation, obtain distillate; Once more, will slip out liquid and concentrate, 100～110 ℃ of thickening temperatures, when the liquid concentrator volume be effluent volume 1/3 ~ 1/4 the time, take out liquid concentrator, add sodium hydroxide solution after cooling and regulate pH=11, obtain spissated distillate; At last, spissated distillate is added chloroform extract, extraction liquid is used anhydrous sodium sulfate dehydration, obtains thick nicotinic solution;
B, pure nicotine preparation method
The thick nicotinic that is obtained among the step a or purity are not less than 60% commercialization thick nicotinic, are that 4.5 ~ 6.5 kPa, temperature are that underpressure distillation is purified, and obtains pure nicotine under 160～170 ℃ the condition at pressure; Under adopting the condition of nitrogen protection, be loaded in the brown container of handling through sterilizing-drying, under the condition of lucifuge, leave in 0 ℃ ~ 4 ℃ the refrigerator and preserve.
2. the preparation method of nicotine reference material according to claim 1 is characterized in that: the brown container described in the step b is made up of the brown ampoule of several 1.0 mL.
3. the preparation method of nicotine reference material according to claim 1 is characterized in that: the standard value of described nicotine reference material and uncertainty thereof are
.
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| CN201210319785XA CN102796076A (en) | 2012-09-03 | 2012-09-03 | Preparation method for nicotine standard substance |
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| CN201210319785XA CN102796076A (en) | 2012-09-03 | 2012-09-03 | Preparation method for nicotine standard substance |
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Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103063489A (en) * | 2012-12-24 | 2013-04-24 | 四川农业大学 | Extraction method of nicotine with diffusion cell |
| CN105566289A (en) * | 2014-10-14 | 2016-05-11 | 北京本草通汇科技中心 | Preparation method of high purity nicotine |
| CN108254233A (en) * | 2017-12-29 | 2018-07-06 | 国家烟草质量监督检验中心 | A kind of nicotine solution standard substance and its preparation method and application |
| CN109738557A (en) * | 2018-12-21 | 2019-05-10 | 国家烟草质量监督检验中心 | A kind of preparation method of nicotine solution standard substance |
| CN109738556A (en) * | 2018-12-21 | 2019-05-10 | 国家烟草质量监督检验中心 | A kind of preparation method of nicotine standard substance and its nicotine standard substance of preparation |
| CN110511210A (en) * | 2019-09-12 | 2019-11-29 | 许达勇 | High purity nicotine production technology |
| CN112704258A (en) * | 2021-01-13 | 2021-04-27 | 江苏鑫源烟草薄片有限公司 | Method for preparing reconstituted tobacco by papermaking method by using multi-element complex and reconstituted tobacco |
| CN112850751A (en) * | 2021-01-09 | 2021-05-28 | 西北大学 | Method for recovering sodium sulfate in nicotine purification process |
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| US3147199A (en) * | 1964-09-01 | Steam |
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Patent Citations (1)
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| US3147199A (en) * | 1964-09-01 | Steam |
Non-Patent Citations (2)
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| 储志兵 等: "高纯度烟碱的制备", 《应用化工》 * |
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Cited By (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103063489A (en) * | 2012-12-24 | 2013-04-24 | 四川农业大学 | Extraction method of nicotine with diffusion cell |
| CN103063489B (en) * | 2012-12-24 | 2015-04-08 | 四川农业大学 | Extraction method of nicotine with diffusion cell |
| CN105566289A (en) * | 2014-10-14 | 2016-05-11 | 北京本草通汇科技中心 | Preparation method of high purity nicotine |
| CN105566289B (en) * | 2014-10-14 | 2018-10-16 | 北京本草通汇科技中心 | A kind of preparation method of high purity nicotine |
| CN108254233A (en) * | 2017-12-29 | 2018-07-06 | 国家烟草质量监督检验中心 | A kind of nicotine solution standard substance and its preparation method and application |
| CN109738557A (en) * | 2018-12-21 | 2019-05-10 | 国家烟草质量监督检验中心 | A kind of preparation method of nicotine solution standard substance |
| CN109738556A (en) * | 2018-12-21 | 2019-05-10 | 国家烟草质量监督检验中心 | A kind of preparation method of nicotine standard substance and its nicotine standard substance of preparation |
| CN110511210A (en) * | 2019-09-12 | 2019-11-29 | 许达勇 | High purity nicotine production technology |
| CN112850751A (en) * | 2021-01-09 | 2021-05-28 | 西北大学 | Method for recovering sodium sulfate in nicotine purification process |
| CN112704258A (en) * | 2021-01-13 | 2021-04-27 | 江苏鑫源烟草薄片有限公司 | Method for preparing reconstituted tobacco by papermaking method by using multi-element complex and reconstituted tobacco |
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Application publication date: 20121128 |