CN104330514B - Combined gas chromatography mass spectrometry combines the method for gas chromatography determination nicotine purity - Google Patents
Combined gas chromatography mass spectrometry combines the method for gas chromatography determination nicotine purity Download PDFInfo
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Abstract
The invention discloses a kind of method that combined gas chromatography mass spectrometry combines gas chromatography determination nicotine purity.First by the purity of GC/MS method Preliminary Determination nicotine, then measuring the moisture content in nicotine by GC method, finally by revising the accurate purity obtaining nicotine, correction formula is as follows: NIC%=nic%* (100% wat%).The method, compared with silico-tungstic acid gravimetric method, has simplicity, quick, easily operated, reproducible feature.High to nicotine detection specificity, it is susceptible in sample the interference of other impurity especially alkaline impurities (alkaloid, inorganic base), when the sample being 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.
Description
Technical field
The invention belongs to the technical field of Nicotiana tabacum L. and tobacco product quality evaluation and mensuration, specifically
Relate to a kind of GC-MS and combine the side of gas chromatography determination nicotine purity
Method.
Technical background
Nicotine (has another name called nicotine, English entitled nicotine), to vegetative nerve and maincenter god
The effect of paralysis after having first excitement, is one of the important component of Nicotiana tabacum L. and tobacco product, is also
Weigh an important indicator in Nicotiana tabacum L. and tobacco product quality control.Meanwhile, nicotine can be used for
The production of the products such as medicine, biological pesticide, cigaret additive, catalyst.Therefore, to nicotine
Analysis, the especially mensuration of nicotine purity, be not only related to the quality of Nicotiana tabacum L. and tobacco product
Control, and comprehensive utilization, nicotine and the derivant thereof of waste/hypo-tobacco leaf developed profit further
With, significant.
The method of domestic and international wide variety of nicotine purity testing is ISO 13276:1997 " cigarette
Grass and the mensuration silico-tungstic acid gravimetric method of tobacco product nicotine purity ", utilize nicotine and water vapour
The principle of azeotropic, in the basic conditions, takes out of nicotine with water vapour, then with silico-tungstic acid
(SiO2·12WO3·26H2O) form crystalline precipitate, precipitation is placed in 120 DEG C of calcinations in baking oven
To constant weight, obtain the content of nicotine by gravimetric method.This method can obtain accurate result, but
There is certain limitation: analysis time is longer；Cannot distinguish between nicotine and nornicotine, measurement result
It it is the summation of two kinds of materials；When in solution containing inorganic salts such as ammonium salts, precipitation is not easily formed,
Interference detection results.
Summary of the invention
Present invention aims to the deficiencies in the prior art, it is provided that a kind of easy and simple to handle, no
Easily by impurity interference, testing result nicotine method for detecting purity the most accurately.
The purpose of the present invention is achieved through the following technical solutions.
Except as otherwise noted, percent of the present invention is mass percent.
A kind of gas chromatography-mass spectrography (GC/MS) method combines gas chromatogram (GC) method and surveys
The method determining nicotine purity, specifically comprises the following steps that
(1) using after nicotine diluted sample 80～120 times as sample to be tested, sample is loaded
In chromatogram bottle, upper machine carries out GC/MS mensuration；
(2) measure with area normalization method and remove on the peak area of nicotine in sample and chromatogram
The area summation of all chromatographic peaks beyond solvent peak, calculates nicotine peak area in sample by Formulas I
Account for the percentage rate of total peak area；
Nic%=Anic/Ai*100………………(I)；
In formula, nic% is the percentage rate that in sample, nicotine peak area accounts for total peak area；
AnicPeak area for nicotine；
AiTotal for removing the area of all chromatographic peaks beyond solvent peak on chromatogram
With；
(3), after taking nicotine sample isopropanol and adding internal standard, gas chromatogram GC is used
Method measures its moisture content, is designated as wat%；
(4) the nicotine Reinheitszahl NIC% of sample it is calculated by 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 percentage rate that in sample, nicotine peak area accounts for total peak area；
Wat% is the moisture content of sample.
In step (1), conventional the having of the gas chromatogram such as nicotine sample isopropanol or hexamethylene
Machine solvent dilution obtains sample to be tested.In order to prevent the contingent reaction of nicotine, as aoxidized,
Degraded, the moisture absorption etc., the diluent of nicotine solution should configure before measuring, and i.e. join and i.e. use；
In step (3), precise nicotine sample 100mg, it is accurate to 0.1mg, places
In the volumetric flask of 10mL, do interior target isopropyl alcohol extraction with containing 5mL/L dehydrated alcohol
Agent constant volume, after mix homogeneously, loads in chromatogram bottle；Then GB/T 23203.1-2008 is used
The method of " the mensuration part 1 of moisture in Cigarette grain phase: gas chromatography " measures
Contained 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 equivalence chromatographic columns；
B, sample size: 1.0 μ L；
C, solvent clipping time: 5min；
D, injector temperature: 250 DEG C；
E, temperature programming condition: initial temperature 100 DEG C, rise 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；Last with 20 DEG C/min
Rise to 220 DEG C, 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 is arranged :-70eV；Scan mode is full scan；
Sweep limits: 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 equivalence 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 detector: temperature 250 DEG C.
The present invention during nicotine content mensuration, is used for marking be applicable to Nicotiana tabacum L., tobacco product and flue gas
Nicotine that quasi-analysis method is used or the purity testing of nicotine salt.With the most wide variety of
ISO 13276:1997 " the mensuration silico-tungstic acid gravimetric method of Nicotiana tabacum L. and tobacco product nicotine purity "
Compare, there is simplicity, quick, easily operated, reproducible feature.Meanwhile, the method
Utilize modern chromatographic techniques sample is carried out after high efficiency separation again with the intrinsic physicochemical constant of nicotine it
The molecular weight of one is as detection target, high to nicotine detection specificity, is susceptible in sample other
The interference of impurity especially alkaline impurities (alkaloid, inorganic base), to nicotine sample especially
Be be long placed in, sample that impurity content is higher is when carrying out purity detecting, easy and simple to handle, separating power
By force, 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.
Detailed description of the invention
In order to be more fully understood that the present invention, with embodiment, the present invention is done into one below in conjunction with the accompanying drawings
The detailed description of step, but drawings and Examples are not limited to the technical solution.
Embodiment 1:
(1) material and instrument:
(1) reagent: hydrochloric acid (AR, Chemical Co., Ltd. in pairs of Yantai City)；Silico-tungstic acid (AR,
Shanghai reagent two factory)；Isopropanol (chromatographically pure, TEDIA Company, Inc. company)；
Dehydrated alcohol (AR, Shanghai reagent one factory)；
(2) instrument: Motto-Q Superpure water machine (Millipore company)；AG204 electronics
Balance (sensibility reciprocal: 0.0001g, METTLER TOLEDO company of Switzerland)；Air blast constant temperature
Drying baker (101A-2, Shanghai City experimental apparatus head factory)；(5975, Agilent is public for GC/MS
Department)；GC (7890, Agilent company)；Quantitative charger (Brand company of Germany)；
Liquid-transfering gun (Tripette company).
(2) preparation of sample and the mensuration of nicotine purity:
(1) purity nic% of GC/MS method Preliminary Determination nicotine
Prepared by A, sample: by nicotine sample A (being long placed in sample) isopropanol 100 times
As sample to be tested, i.e. take nicotine sample A 0.1mL, be placed in the volumetric flask of 10mL,
Use isopropanol constant volume, after mix homogeneously, 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 equivalence chromatographic columns, such as DB-5MS quartz capillary column (30m
×0.25mm×0.25μm)、(30m×0.25mm×0.25μm)
Deng；
B) sample size: 1.0 μ L；If detector or the saturated situation of chromatographic column occur, permissible
The most suitably reduce sample size；
C) solvent clipping time: 5min；Can be suitable according to selected temperature programming condition
When adjusting solvent clipping time；
D) injector temperature: 250 DEG C；
E) temperature programming 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；Last with 20 DEG C/min
Rise to 220 DEG C, keep 10min；Other can be selected suitable according to the concrete condition of sample
Temperature programming condition；
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 is arranged :-70eV；Scan mode is full scan；Sweep
Retouch scope: m/z=29-500.
C, the calculating of measurement result: measure the face, peak of each component in sample with area normalization method
Remove the area of total chromatographic peak beyond solvent peak on long-pending and chromatogram, calculate nicotine peak area and account for
The percentage rate of total peak area, i.e. can get the content of nicotine；By the content of all components in sample
Sum is set to 100%, and the method calculating wherein a certain component is:
xi%=fiAi/(fiAi)*100………………①
Wherein, xiFor the percentage composition of component i in sample；
fiCorrection factor for component i；
AiFor peak area or the peak height of component i, this method brings calculating into peak area；
Owing to the impurity in nicotine and its main component nicotine are all the alkaloids containing pyridine ring
Compound, close due in structure, their correction factor also approximately equal, can ignore
Correction factor, by direct for area normalization, is calculated by equation below:
xi%=Ai/Ai*100………………②
Utilize formula 2. to calculate nicotine peak area and account for the percentage rate of total peak area, containing of available nicotine
Amount, it may be assumed that
Nic%=Anic/Ai*100………………(I)
Wherein, the percentage composition (not considering that moisture affects) of nicotine during nic% is sample；
AnicPeak area for nicotine；
AiTotal for removing the area of all chromatographic peaks beyond solvent peak on chromatogram
With.
D, nicotine sample A prepare 7 parts of dilute solutions according to the method described above, use GC-MS respectively
Method measures its nicotine content, spectrogram as it is shown in figure 1, measured value is followed successively by 98.66%, 98.64%,
95.57%, 98.64%, 98.56%, 98.54%, 98.53%, measuring meansigma methods is 98.59%,
SD is 0.05.
Nearly ten years, instrument analysis technology quickly grows, and achieves rapid progress.Especially color
The development of spectrum-mass spectrometric hyphenated technique, the new method for research nicotine purity testing provides effectively
Technical support.Owing to chromatographic technique has high separability energy, nicotine can be divided with other components
From, thus reduce the interference that nicotine content is measured by remaining component.Simultaneously as mass spectrum skill
Art measures the molecular weight of one of compound fundamental nature, and testing result is the most directly perceived, accurately.Cause
This, chromatograph-mass spectrometer coupling technology has a good application prospect in terms of nicotine content mensuration.
Although, chromatography has preferable separating effect to the component in testing sample, but, its
The self property of detector, there is also certain limitation: configure ultraviolet (UV) detector
Or moisture is not responded to by the chromatograph of liquid (LC) of fluorescence detector (FLD)；Meanwhile,
GC, LC/MS, GC/MS isochrome spectrometer of configuration mass spectrum (MS) detector, owing to treating
Test sample product can accept the process of dehydration before entering MS detector, in order to protect MS detector.
Thus, the nicotine content that these methods are measured all can not embody the moisture shadow to measurement result
Ringing, i.e. there is method error bigger than normal in measured value.
The nicotine being long placed in the moisture absorption can cause water content to rise, and nicotine purity declines.When moisture content reaches
During to 2%-5%, the impact of nicotine purity can not be left in the basket by it, thus, it is necessary to cigarette
Moisture in alkali is measured, and the nicotine content value measuring GC/MS method is modified.
Moisture in GC internal mark method determination nicotine and the like sample is a kind of technology maturation, operation
Easy, the method for reliable results, therefore, in the present invention, uses GB/T 23203.1-2008
The method of " the mensuration part 1 of moisture in Cigarette grain phase: gas chromatography " measures
Moisture contained in nicotine sample.
Based on this, the present invention is first with GC/MS method Preliminary Determination nicotine content, recycling
GC internal mark method determination sample moisture content, finally, obtains accurate cigarette by data analysis
Alkali purity data.With currently used classical way ISO 13276:1997 " Nicotiana tabacum L. and cigarette
The mensuration silico-tungstic acid gravimetric method of straw-made articles nicotine purity " compare, the method tool of the present invention
Have simple and efficient, easily operated, reproducible feature, have important significance of scientific research with relatively
High using value, is called for short GC/MS-GC method.
(2) moisture wat% contained during GC method measures nicotine sample.
Prepared by A, sample: precise nicotine sample A 100mg, is accurate to 0.1mg, puts
It is placed in the volumetric flask of 10mL, does interior target isopropanol extraction with containing 5mL/L dehydrated alcohol
Take agent constant volume, after mix homogeneously, load in chromatogram bottle to be measured；
B, use the GB/T 23203.1-2008 " mensuration the 1st of moisture in Cigarette grain phase
Part: gas chromatography " method measure moisture contained in nicotine sample.
C, measurement result:
Nicotine sample A is prepared for 3 parts of dilute solutions according to described method, uses GC method respectively
Measuring its nicotine moisture content, as shown in table 1, its moisture content is followed successively by 2.41%, 2.34% and
2.47%, meansigma methods is 2.41%, and SD is 0.06.
Table 1GC method measures the result of nicotine moisture content (wat%)
(3) GC/MS-GC method nicotine purity testing result calculates
Based on said determination result, bring equation 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 percentage rate that in sample, nicotine peak area accounts for total peak area；
Wat% is the moisture content 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 (freshly prepared sample), system
Standby 7 parts of dilute solutions, measure its nicotine content by GC-MS method, spectrogram as in figure 2 it is shown,
Measured value is followed successively by 99.53%, 99.53%, 99.46%, 99.64%, 99.51%, 99.56%,
99.58%, measuring meansigma methods is 99.54%, and SD is 0.06；Its moisture content and meansigma methods thereof and
GC/MS-GC method measures the result of nicotine purity (NIC%) the most 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), preparation
4 parts of dilute solutions, measure its nicotine content by GC-MS method, spectrogram as it is shown on figure 3,
Measured value is followed successively by 99.05%, 99.01%, 99.06%, 99.01%, measures meansigma methods and is
99.03%, SD are 0.03.Its moisture content and meansigma methods and GC/MS-GC method thereof measure nicotine
The result of purity (NIC%) is the most as shown in Table 1 and Table 2.
Embodiment 4:
Use ISO 13276:1997 " Nicotiana tabacum L. and the mensuration silico-tungstic acid of tobacco product nicotine purity
Gravimetric method " measure nicotine sample A, B and C purity, result is as shown in table 3.
The result of table 3 silico-tungstic acid gravimetric detemination nicotine purity
It is close that silico-tungstic acid gravimetric method and GC/MS-GC method of the present invention measure nicotine purity result,
Fig. 4 embodies both relations intuitively, indicate the inventive method measure nicotine purity can
By property.
From Fig. 1～4 and table 1～3, result that embodiment 1～3 is measured and silico-tungstic acid
Gravimetric method is compared, measurement result is not significantly different from, it was demonstrated that the method for the invention accurate
Feasibility.Respectively group data understand: enter for freshly prepared nicotine sample (sample B)
When row nicotine content measures, silico-tungstic acid gravimetric method and GC/MS-GC method is utilized to record result base
This is identical, respectively 99.34% and 99.54%；And to being long placed in sample (sample A and C)
Finding when detecting, the result of silico-tungstic acid gravimetric method gained measures than GC/MS-GC method
Lower result.In order to analyze the reason producing above-mentioned difference, we are to being long placed in impurity in sample
Constitute and analyzed, found that such impurity mainly includes dehydrogenation nornicotine, diene
Nicotine and methyl anabasine, this is owing to nicotine can occur the moisture absorption, degraded in placement process
With isomerization, generate nicotine derivative and/or the peculiar alkaloid of other Nicotiana tabacum L.s.Based on above real
Test result, it is presumed that, it is of a relatively high owing to being long placed in nicotine derivative impurity content in sample,
Such alkaloid compound can hinder nicotine and salt thereof and the combination of silico-tungstic acid and precipitation, because of
When this utilizes silico-tungstic acid gravimetric method to carry out purity detecting, due to other types alkaloid and/or its
The interference of his impurity, nicotine cannot become salt to precipitate completely, cause measured value more smaller than actual value.
And on the other hand, owing to GC/MS method directly detects the build-in attribute molecular weight of nicotine,
Its measurement result is affected less by remaining alkaloid impurity, and therefore, its measured value should be with reality
Value is more closely, the numerical value utilizing GC/MS-GC method to measure should be greater than silico-tungstic acid weight simultaneously
Method gained measured value.Our experimental result is also consistent with above-mentioned supposition: when sample is freshly prepared
Time (sample B), owing in sample, nicotine goes bad less, therefore, two kinds of methods record respectively
Nicotine content numeric ratio be closer to；When to be long placed in sample (sample A and C) detect time,
In sample, nicotine goes bad more, and silico-tungstic acid gravimetric method is detected number by remaining alkaloid consequent
According to causing certain impact, it is allowed to less than actual content.And owing to GC/MS-GC method is not subject to
Remaining alkaloid disturbs, so, utilize this method gained measured value to be more nearly actual value and be more than
Silico-tungstic acid gravimetric method detected value.Therefore, GC/MS-GC method is compared to silico-tungstic acid gravimetric method more
Easy, accurately.
Claims (1)
1. the method that combined gas chromatography mass spectrometry combines gas chromatography determination nicotine purity, bag
Include following steps:
(1) using after nicotine diluted sample 80～120 times as sample to be tested, sample is loaded chromatogram bottle
On in, machine carries out GC/MS mensuration；The chromatographic condition that GC/MS measures is specific as follows:
A, chromatographic column: hp-5MS quartz capillary column, specification 30m × 0.25mm × 0.25
μm, or other equivalence chromatographic columns；
B, sample size: 1.0 μ L；
C, solvent clipping time: 5min；
D, injector temperature: 250 DEG C；
E, temperature programming condition: initial temperature 100 DEG C, rise 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, protect
Hold 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 is arranged :-70eV；Scan mode is full scan；Sweep limits:
M/z=29-500；
(2) measure with area normalization method and remove solvent peak on the peak area of nicotine in sample and chromatogram
The area summation of all chromatographic peaks in addition, calculates nicotine peak area in sample by Formulas I and accounts for total peak area
Percentage rate；
Nic%=Anic/Ai*100………………(I)；
In formula, nic% is the percentage rate that in sample, nicotine peak area accounts for total peak area；
AnicPeak area for nicotine；
AiFor removing the area summation of all chromatographic peaks beyond solvent peak on chromatogram；
(3), after taking nicotine sample isopropanol and adding internal standard, measure by gas chromatogram GC method
Its moisture content, is designated as wat%；The chromatographic condition that GC measures is specific as follows:
A, chromatographic column: HP-PLOT/Q capillary chromatographic column, specification 30m × 0.32mm × 0.25 μm,
Or other equivalence 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 detector: temperature 250 DEG C；
(4) the nicotine Reinheitszahl NIC% of sample it is calculated by 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 percentage rate that in sample, nicotine peak area accounts for total peak area；
Wat% is the moisture content of sample.
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| NL2032578A (en) * | 2022-07-22 | 2022-09-28 | Yunnan Tobacco Quality Supervision And Testing Station | Method for Determining Purity of Nicotine by Use of GCMS-GC Method |
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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 |
| 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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