CN104330514A - Method for measuring nicotine purity by combination of gas chromatography-mass spectrometry method in combination with gas chromatographic method - Google Patents
Method for measuring nicotine purity by combination of gas chromatography-mass spectrometry method in combination with gas chromatographic method Download PDFInfo
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Abstract
The invention discloses a method for measuring nicotine purity combination of a gas chromatography-mass spectrometry method and a gas chromatographic method. The purity of the nicotine is preliminarily measured by use of the GC-MS method, next, the moisture content in the nicotine is measured by use of the GC method, and finally, the accurate purity of the nicotine is obtained by virtue of correction according to a correction formula NIC%=nic%*(100%-wat%). Compared with a silicotungstic acid weight method, the method has the characteristics of being simple and convenient, fast, easy to operate and good in repeatability. The method is high in nicotine detection specificity, and is not affected by other impurities, in particular alkaline impurities (alkaloid and inorganic bases), in the sample; during purity detection on the nicotine sample, in particular a sample which is arranged for a long time and is high in impurity content, the method is simple and convenient to operate, and high in separation capacity, and the qualitative and quantitative results are reliable.
Description
Technical field
The invention belongs to the technical field of tobacco and tobacco product quality assessment and mensuration, specifically relate to the method for a kind of GC-MS(gas chromatography-mass spectrography) in conjunction with gas chromatography determination nicotine purity.
Technical background
Nicotine (has another name called nicotine, English nicotine by name), vegetative nerve and nervous centralis being had to the effect of first excited rear paralysis, is one of important component of tobacco and tobacco product, is also weigh an important indicator in tobacco and tobacco product quality control.Meanwhile, nicotine can be used for the production of the products such as medicine, biological pesticide, cigarette additive, catalyzer.Therefore, to the analysis of nicotine, the especially mensuration of nicotine purity, is not only related to the quality control of tobacco and tobacco product, and the further exploitation to the comprehensive utilization of waste/hypo-tobacco leaf, nicotine and derivant thereof, significant.
The method of the nicotine purity testing of domestic and international widespread use is ISO 13276:1997 " the mensuration silico-tungstic acid gravimetric method of tobacco and tobacco product nicotine purity ", utilize the principle of nicotine and water vapour azeotropic, in the basic conditions, with water vapour, nicotine is taken out of, then with silico-tungstic acid (SiO
212WO
326H
2o) form crystalline precipitate, precipitation is placed in 120 DEG C of calcinations in baking oven and, to constant weight, obtains the content of nicotine by gravimetric method.This method can obtain result more accurately, but has certain limitation: analysis time is longer; Can not distinguish nicotine and nornicotine, measurement result is the summation of two kinds of materials; When containing the inorganic salts such as ammonium salt in solution, precipitation is not easily formed, interference detection results.
Summary of the invention
The object of the invention is to for the deficiencies in the prior art, provide a kind of easy and simple to handle, be not subject to impurity interference, testing result nicotine method for detecting purity more accurately.
Object of the present invention is achieved through the following technical solutions.
Except as otherwise noted, percentage of the present invention is mass percent.
A kind of gas chromatography-mass spectrography (GC/MS) method measures the method for nicotine purity in conjunction with gas chromatography (GC) method, concrete steps are as follows:
(1) using after nicotine Sample Dilution 80 ~ 120 times as sample to be tested, sample to be loaded in chromatogram bottle machine and carries out GC/MS mensuration;
(2) the peak area of nicotine in area normalization method measurement sample and chromatogram to remove the area summation of all chromatographic peaks beyond solvent peak, the percent of total peak area is accounted for nicotine peak area in formula I calculation sample;
nic％＝A
nic/A
i*100………………(I)；
In formula, nic% is the percent that in sample, nicotine peak area accounts for total peak area;
A
nicfor the peak area of nicotine;
A
ifor chromatogram removing the area summation of all chromatographic peaks beyond solvent peak;
(3) get nicotine sample isopropanol and after adding interior mark, measure its water percentage by gas chromatography GC method, be designated as wat%;
(4) the nicotine Reinheitszahl NIC% of sample is calculated with formula II:
NIC％＝nic％*(100％-wat％)………………(II)；
In formula, NIC% is the percentage composition of nicotine in sample, is the nicotine purity of sample;
Nic% is the percent that in sample, nicotine peak area accounts for total peak area;
Wat% is the water percentage of sample.
In step (1), the organic solvent diluting that the gas chromatographies such as nicotine sample isopropyl alcohol or cyclohexane are commonly used obtains sample to be tested.In order to prevent the contingent reaction of nicotine, as oxidation, degraded, the moisture absorption etc., the dilution of nicotine solution should configure before measuring, and namely joins and namely use;
In step (3), precise nicotine sample 100mg, is accurate to 0.1mg, is positioned in the volumetric flask of 10mL, with doing interior target isopropyl alcohol extraction agent constant volume containing 5mL/L absolute ethyl alcohol, after mixing, loads in chromatogram bottle; Then adopt the method for GB/T 23203.1-2008 " in Cigarette grain phase the mensuration part 1 of moisture: vapor-phase chromatography " measure contained by moisture wat%.
GC/MS described in step (1) measures, and the chromatographic condition of employing is specific as follows:
A, chromatographic column: hp-5MS quartz capillary column (30m × 0.25mm × 0.25 μm), or other equivalent chromatographic columns;
B, sample size: 1.0 μ L;
C, solvent clipping time: 5min;
D, injector temperature: 250 DEG C;
E, temperature programme condition: initial temperature 100 DEG C, rises to 115 DEG C with 0.5 DEG C/min, keep 5min; Then rise to 200 DEG C with 5 DEG C/min, keep 2min; Finally rise to 220 DEG C with 20 DEG C/min, keep 10min;
F, ion source temperature: 230 DEG C;
G, auxiliary region temperature, i.e. interface temperature: 280 DEG C;
H, carrier gas: He (purity >=99.99%);
I, Mass Spectrometry Conditions: EI source; Tuning setting :-70eV; Scan mode is full scan; Sweep limit: m/z=29-500.
GC described in step (3) measures, and the chromatographic condition of employing is specific as follows:
A, chromatographic column: HP-PLOT/Q capillary chromatographic column (30m × 0.32mm × 0.25 μm) or other equivalent chromatographic columns;
B, sample size: 0.5 μ L;
C, injector temperature: 250 DEG C; Split ratio: 10:1;
D, constant temperature 170 DEG C, keeps 10min;
E, TCD detecting device: temperature 250 DEG C.
When the present invention is applicable to nicotine content mensuration in tobacco, tobacco product and flue gas, the nicotine used for standard method of analysis or the purity testing of nicotine salt.Compared with the ISO 13276:1997 " the mensuration silico-tungstic acid gravimetric method of tobacco and tobacco product nicotine purity " of domestic and international widespread use, have easy, quick, be easy to operate, reproducible feature.Simultaneously, the method after utilizing modern chromatographic techniques to be efficiently separated sample again using the molecular weight of one of the intrinsic physicochemical constant of nicotine as detection target, high to nicotine detection specificity, be not subject to the interference of the especially alkaline impurities (alkaloid, inorganic base) of other impurity in sample, when the sample be especially long placed in nicotine sample, impurity content is higher carries out purity detecting, easy and simple to handle, separating power is strong, qualitative, quantitative reliable results.
Accompanying drawing explanation
Fig. 1 is that the GC/MS method of sample A measures nicotine content spectrogram;
Fig. 2 is that the GC/MS method of sample B measures nicotine content spectrogram;
Fig. 3 is that the GC/MS method of sample C measures nicotine content spectrogram;
Fig. 4 is the results contrast of silico-tungstic acid gravimetric method and GC/MS-GC method of the present invention.
Embodiment
In order to understand the present invention better, below in conjunction with drawings and Examples, the present invention is described in further detail, but drawings and Examples are not limited to the technical solution.
Embodiment 1:
(1) material and instrument:
(1) reagent: hydrochloric acid (AR, Yantai City is Chemical Co., Ltd. in pairs); Silico-tungstic acid (AR, Shanghai reagent two factory); Isopropyl alcohol (chromatographically pure, TEDIA Company, Inc. company); Absolute ethyl alcohol (AR, Shanghai reagent one factory);
(2) instrument: Motto-Q Superpure water machine (Millipore company); AG204 electronic balance (sensibility reciprocal: 0.0001g, METTLER TOLEDO company of Switzerland); Air blast thermostatic drying chamber (101A-2, Shanghai City experimental apparatus head factory); GC/MS (5975, Agilent company); GC (7890, Agilent company); Quantitative charger (German Brand company); Liquid-transfering gun (Tripette company).
(2) preparation of sample and the mensuration of nicotine purity:
(1) the purity nic% of GC/MS method Preliminary Determination nicotine
A, sample preparation: use isopropanol 100 doubly as sample to be tested nicotine sample A (being long placed in sample), namely get nicotine sample A 0.1mL, be placed in the volumetric flask of 10mL, use isopropyl alcohol constant volume, after mixing, load in chromatogram bottle;
B, when GC/MS measures, the chromatographic condition of employing is specific as follows:
A) chromatographic column: hp-5MS quartz capillary column (30m × 0.25m × 0.25 μm); Or other equivalent chromatographic columns, as DB-5MS quartz capillary column (30m × 0.25mm × 0.25 μm),
(30m × 0.25mm × 0.25 μm) etc.;
B) sample size: 1.0 μ L; If there is detecting device or the saturated situation of chromatographic column, optionally suitably sample size can be reduced;
C) solvent clipping time: 5min; Can according to selected temperature programme condition, suitably adjustment solvent clipping time;
D) injector temperature: 250 DEG C;
E) temperature programme condition: initial temperature 100 DEG C, rises to 115 DEG C with 0.5 DEG C/min, keeps 5min; Then rise to 200 DEG C with 5 DEG C/min, keep 2min; Finally rise to 220 DEG C with 20 DEG C/min, keep 10min; Can concrete condition per sample, the temperature programme condition selecting other suitable;
F) ion source temperature: 230 DEG C;
G) auxiliary region temperature, i.e. interface temperature: 280 DEG C;
H) carrier gas: He (purity >=99.99%);
I) Mass Spectrometry Conditions: EI source; Tuning setting :-70eV; Scan mode is full scan; Sweep limit: m/z=29-500.
The calculating of C, measurement result: the peak area of each component in area normalization method measurement sample and chromatogram to remove the area of the total chromatographic peak beyond solvent peak, calculate the percent that nicotine peak area accounts for total peak area, the content of nicotine can be obtained; The content sum of all components in sample is decided to be 100%, and the method calculating wherein a certain component is:
x
i％＝f
iA
i/(f
iA
i)*100………………①
Wherein, x
ifor the percentage composition of component i in sample;
F
ifor the correction factor of component i;
A
ifor peak area or the peak height of component i, in this method, bring calculating into peak area;
Due to the alkaloid compound that the impurity in nicotine and its principal ingredient nicotine are all containing pyridine ring, due to structural close, their correction factor also approximately equal, can ignore correction factor, by direct for area normalization, and the formulae discovery by below:
x
i％＝A
i/A
i*100………………②
Utilize formula 2. to calculate percent that nicotine peak area accounts for total peak area, can obtain the content of nicotine, that is:
nic％＝A
nic/A
i*100………………(I)
Wherein, nic% is the percentage composition (not considering moisture effects) of nicotine in sample;
A
nicfor the peak area of nicotine;
A
ifor chromatogram removing the area summation of all chromatographic peaks beyond solvent peak.
D, nicotine sample A prepare 7 parts of dilute solutions according to the method described above, its nicotine content is measured respectively by GC-MS method, spectrogram as shown in Figure 1, measured value is followed successively by 98.66%, 98.64%, 95.57%, 98.64%, 98.56%, 98.54%, 98.53%, mensuration mean value is 98.59%, SD is 0.05.
Nearly ten years, instrument analysis technology development rapidly, achieves rapid progress.Especially the development of chromatograph-mass spectrometer coupling technology, for the new method of research nicotine purity testing provides strong technical support.Because chromatographic technique has high separability energy, can by nicotine and other Component seperation, thus reduce the interference that all the other components measure nicotine content.Meanwhile, because mass-spectrometric technique measures the molecular weight of one of compound fundamental nature, testing result is more directly perceived, accurate.Therefore, chromatograph-mass spectrometer coupling technology has a good application prospect in nicotine content mensuration.
Although, chromatography has good separating effect to the component in testing sample, but, the self property of its detecting device, also has some limitations: the liquid chromatograph (LC) of configuration ultraviolet (UV) detecting device or fluorescence detector (FLD) does not respond moisture; Meanwhile, GC, LC/MS, GC/MS isochrome spectrometer of configuration mass spectrum (MS) detecting device, because testing sample can accept the process of dehydration, in order to protect MS detecting device before entering MS detecting device.Thus, the nicotine content that these methods measure all can not embody the impact of moisture on measurement result, and namely measured value exists method error bigger than normal.
The nicotine be long placed in can the moisture absorption cause water cut to rise, and nicotine purity declines.When water percentage reaches 2%-5%, it can not be left in the basket on the impact of nicotine purity, thus, is necessary to measure the moisture in nicotine, and revises the nicotine content value that GC/MS method measures.Moisture in GC internal mark method determination nicotine and analog sample thereof is a kind of method of technology maturation, easy and simple to handle, reliable results, therefore, in the present invention, the method for GB/T 23203.1-2008 " in Cigarette grain phase the mensuration part 1 of moisture: vapor-phase chromatography " is adopted to measure moisture contained in nicotine sample.
Based on this, first the present invention utilizes GC/MS method Preliminary Determination nicotine content, and recycling GC internal mark method determination sample moisture content, finally, obtains nicotine purity data comparatively accurately by data analysis.Compared with the classical way---ISO 13276:1997 " the mensuration silico-tungstic acid gravimetric method of tobacco and tobacco product nicotine purity "---used at present, method of the present invention have simple and efficient, be easy to operate, reproducible feature, there is important significance of scientific research and higher using value, be called for short GC/MS-GC method.
(2) GC method measures moisture wat% contained in nicotine sample.
A, sample preparation: precise nicotine sample A 100mg, is accurate to 0.1mg, is positioned in the volumetric flask of 10mL, with doing interior target isopropyl alcohol extraction agent constant volume containing 5mL/L absolute ethyl alcohol, after mixing, load in chromatogram bottle to be measured;
B, the method for GB/T 23203.1-2008 " in Cigarette grain phase the mensuration part 1 of moisture: vapor-phase chromatography " is adopted to measure moisture contained in nicotine sample.
C, measurement result:
Nicotine sample A has prepared 3 parts of dilute solutions according to described method, and measure its nicotine water percentage by GC method respectively, as shown in table 1, its water percentage is followed successively by 2.41%, 2.34% and 2.47%, and mean value is 2.41%, SD is 0.06.
Table 1GC method measures the result of nicotine water percentage (wat%)
(3) GC/MS-GC method nicotine purity testing result calculates
Based on said determination result, bring formula below into:
NIC％＝nic％*(100％-wat％)………………(II)；
Wherein, NIC% is the percentage composition of nicotine in sample, is the nicotine purity of sample;
Nic% is the percent that in sample, nicotine peak area accounts for total peak area;
Wat% is the water percentage of sample;
Calculate the nicotine purity (NIC%) of sample, as shown in table 2.
Table 2GC/MS-GC method measures the result of nicotine purity (NIC%)
Embodiment 2:
Repeat the process of embodiment 1, select another nicotine sample B (brand-new is for sample), 7 parts of dilute solutions are prepared, its nicotine content is measured by GC-MS method, spectrogram as shown in Figure 2, measured value is followed successively by 99.53%, 99.53%, 99.46%, 99.64%, 99.51%, 99.56%, 99.58%, and mensuration mean value is 99.54%, SD is 0.06; The result of its water percentage and mean value and GC/MS-GC method mensuration nicotine purity (NIC%) respectively as shown in Table 1 and Table 2.
Embodiment 3:
Repeat the process of embodiment 1, select another nicotine sample C (being long placed in sample), 4 parts of dilute solutions are prepared, its nicotine content is measured by GC-MS method, spectrogram as shown in Figure 3, measured value is followed successively by 99.05%, 99.01%, 99.06%, 99.01%, and mensuration mean value is 99.03%, SD is 0.03.The result of its water percentage and mean value and GC/MS-GC method mensuration nicotine purity (NIC%) respectively as shown in Table 1 and Table 2.
Embodiment 4:
Adopt ISO 13276:1997 " the mensuration silico-tungstic acid gravimetric method of tobacco and tobacco product nicotine purity " to measure the purity of nicotine sample A, B and C, result is as shown in table 3.
The result of table 3 silico-tungstic acid gravimetric determination nicotine purity
It is close that silico-tungstic acid gravimetric method and GC/MS-GC method of the present invention measure nicotine purity result, and Fig. 4 embodies both relation intuitively, indicates the reliability that the inventive method measures nicotine purity.
From Fig. 1 ~ 4 and table 1 ~ 3, the result that embodiment 1 ~ 3 measures is compared with silico-tungstic acid gravimetric method, and measurement result does not have significant difference, demonstrates the accurate feasibility of the method for the invention.Carefully respectively organize data known: when nicotine content mensuration is carried out for nicotine sample (sample B) for brand-new, utilize silico-tungstic acid gravimetric method and GC/MS-GC method to record result substantially identical, be respectively 99.34% and 99.54%; And finding being long placed in when sample (sample A and C) detects, the Lower result that the result of silico-tungstic acid gravimetric method gained measures than GC/MS-GC method.In order to analyze the reason producing above-mentioned difference, we analyze being long placed in the formation of impurity in sample, found that such impurity mainly comprises dehydrogenation nornicotine, nicotyrine and methyl anabasine, this is because nicotine, in put procedure, the moisture absorption, degraded and isomerization can occur, and generates nicotine derivative and/or the peculiar alkaloid of other tobaccos.Based on above experimental result, we infer, relatively high owing to being long placed in nicotine derivative impurity content in sample, such alkaloid compound can hinder combination and the precipitation of nicotine and salt and silico-tungstic acid, when therefore utilizing silico-tungstic acid gravimetric method to carry out purity detecting, due to the interference of other types alkaloid and/or other impurity, nicotine cannot salify precipitation completely, causes measured value more smaller than actual value.And on the other hand, due to build-in attribute---the molecular weight of GC/MS method direct-detection nicotine, its measurement result is less by the impact of all the other alkaloid impurity, therefore, its measured value should be more close with actual value, and the numerical value simultaneously utilizing GC/MS-GC method to measure should be greater than silico-tungstic acid gravimetric method gained measured value.Our experimental result also conforms to above-mentioned supposition: when sample be brand-new for time (sample B), because nicotine in sample goes bad less, therefore, the nicotine content numerical value that two kinds of methods record respectively is relatively; When to be long placed in sample (sample A and C) detect time, in sample, nicotine goes bad more, all the other alkaloids consequent to silico-tungstic acid gravimetric method detect data cause certain influence, make it lower than actual content.And do not disturb by all the other alkaloids due to GC/MS-GC method, so, utilize this method gained measured value to be more greater than silico-tungstic acid gravimetric method detected value close to actual value.Therefore, GC/MS-GC method is more easy, accurate compared to silico-tungstic acid gravimetric method.
Claims (3)
1. combined gas chromatography mass spectrometry is in conjunction with a method for gas chromatography determination nicotine purity, comprises the steps:
(1) using after nicotine Sample Dilution 80 ~ 120 times as sample to be tested, sample to be loaded in chromatogram bottle machine and carries out GC/MS mensuration;
(2) the peak area of nicotine in area normalization method measurement sample and chromatogram to remove the area summation of all chromatographic peaks beyond solvent peak, calculate nicotine peak area in sample with formula I and account for the percent of total peak area;
nic％＝A
nic/A
i*100..................(I)；
In formula, nic% is the percent that in sample, nicotine peak area accounts for total peak area;
A
nicfor the peak area of nicotine;
A
ifor chromatogram removing the area summation of all chromatographic peaks beyond solvent peak;
(3) get nicotine sample isopropanol and after adding interior mark, measure its water percentage by gas chromatography GC method, be designated as wat%;
(4) the nicotine Reinheitszahl NIC% of sample is calculated with formula II:
NIC％＝nic％*(100％-wat％)..................(II)；
In formula, NIC% is the percentage composition of nicotine in sample, is the nicotine purity of sample;
Nic% is the percent that in sample, nicotine peak area accounts for total peak area;
Wat% is the water percentage of sample.
2. the method for mensuration nicotine purity according to claim 1, is characterized in that: the GC/MS described in step (1) measures, and the chromatographic condition of employing is specific as follows:
A, chromatographic column: hp-5MS quartz capillary column (30m × 0.25mm × 0.25 μm), or other equivalent chromatographic columns;
B, sample size: 1.0 μ L;
C, solvent clipping time: 5min;
D, injector temperature: 250 DEG C;
E, temperature programme condition: initial temperature 100 DEG C, rises to 115 DEG C with 0.5 DEG C/min, keep 5min; Then rise to 200 DEG C with 5 DEG C/min, keep 2min; Finally rise to 220 DEG C with 20 DEG C/min, keep 10min;
F, ion source temperature: 230 DEG C;
G, auxiliary region temperature, i.e. interface temperature: 280 DEG C;
H, carrier gas: He (purity >=99.99%);
I, Mass Spectrometry Conditions: EI source; Tuning setting :-70eV; Scan mode is full scan; Sweep limit: m/z=29-500.
3. the method for mensuration nicotine purity according to claim 1, is characterized in that: the GC described in step (3) measures, and the chromatographic condition of employing is specific as follows:
A, chromatographic column: HP-PLOT/Q capillary chromatographic column (30m × 0.32mm × 0.25 μm) or other equivalent chromatographic columns;
B, sample size: 0.5 μ L;
C, injector temperature: 250 DEG C; Split ratio: 10:1;
D, constant temperature 170 DEG C, keeps 10min;
E, TCD detecting device: temperature 250 DEG C.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN105067716A (en) * | 2015-07-03 | 2015-11-18 | 江苏中烟工业有限责任公司 | Method for determining puff-by-puff nicotine and tar in cigarette mainstream smoke |
| CN113009046A (en) * | 2021-03-30 | 2021-06-22 | 山东金城医药化工有限公司 | GC-MS-MS detection and analysis method for synthesizing nicotine |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| NL2032578B1 (en) * | 2022-07-22 | 2023-03-31 | Yunnan Tobacco Quality Supervision And Testing Station | Method for Determining Purity of Nicotine by Use of GCMS-GC Method |
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2014
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN105067716A (en) * | 2015-07-03 | 2015-11-18 | 江苏中烟工业有限责任公司 | Method for determining puff-by-puff nicotine and tar in cigarette mainstream smoke |
| CN113009046A (en) * | 2021-03-30 | 2021-06-22 | 山东金城医药化工有限公司 | GC-MS-MS detection and analysis method for synthesizing nicotine |
| CN113009046B (en) * | 2021-03-30 | 2023-10-17 | 山东金城医药化工有限公司 | GC-MS-MS detection and analysis method for synthesizing nicotine |
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