CN106896173B - The chiral analysis of nicotine closes phase chromatographic tandem mass spectrography in a kind of electronic cigarette liquid - Google Patents
The chiral analysis of nicotine closes phase chromatographic tandem mass spectrography in a kind of electronic cigarette liquid Download PDFInfo
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- CN106896173B CN106896173B CN201710141868.7A CN201710141868A CN106896173B CN 106896173 B CN106896173 B CN 106896173B CN 201710141868 A CN201710141868 A CN 201710141868A CN 106896173 B CN106896173 B CN 106896173B
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- G—PHYSICS
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- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
- G01N30/04—Preparation or injection of sample to be analysed
- G01N30/06—Preparation
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
- G01N30/62—Detectors specially adapted therefor
- G01N30/72—Mass spectrometers
- G01N30/7233—Mass spectrometers interfaced to liquid or supercritical fluid chromatograph
- G01N30/724—Nebulising, aerosol formation or ionisation
- G01N30/7266—Nebulising, aerosol formation or ionisation by electric field, e.g. electrospray
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
- G01N30/04—Preparation or injection of sample to be analysed
- G01N30/06—Preparation
- G01N2030/062—Preparation extracting sample from raw material
Abstract
The invention discloses a kind of chiral analysis of nicotine in electronic cigarette liquid to close phase chromatographic tandem mass spectrography.It is characterized by: by electronic cigarette liquid sample after sodium hydroxide solution infiltrates, using methyl tertiary butyl ether(MTBE) and methanol solution extraction, extract liquor is after Dispersive solid phase extraction purifies, it is connected-is closed phase chromatographic tandem analytical reagent composition using two chiral columns, using S- (-)-nicotine in areas of peak normalization method quantitative detection electronic cigarette liquid and R- (+)-nicotine ratio.The detection method that this method provides, sample extraction purification method is simple and efficient, pollution of the sample liquid to chromatographic column can be reduced, close phase chromatographic tandem mass spectrography detection method high sensitivity, specificity is good, false positive can be excluded, analysis time is short, can satisfy the chiral analysis of nicotine in high-volume electronic cigarette liquid sample.
Description
Technical field
The present invention relates to electronic cigarette liquid chemical constituents determination methods, and in particular to the chirality point of nicotine in a kind of electronic cigarette liquid
Phase chromatographic tandem mass spectrography is closed in analysis.
Background technique
Nicotine is also nicotine, is the important component of a kind of alkaloid being present in plant of Solanaceae and tobacco.Cigarette
Base molecule contains a chiral centre, i.e., 2 carbon atoms on nafoxidine ring, so there are two enantiomers for nicotine: S- (-)-
Nicotine and R- (+)-nicotine.Two enantiomers of nicotine have entirely different content, metabolic mechanism and physiological property.It therefore need to be into
The chiral analysis of nicotine in row electronic cigarette liquid.
At present about the chiral analysis of nicotine, mainly studied using gas chromatography, such as application No. is
201610663534.1 patent " a kind of chiral analysis method of nicotine in cigarette shreds ", this method pre-treatment step is complicated,
And detection time reaches 140min, is not able to satisfy the detection of a large amount of samples, and there has been no about nicotine in electronic cigarette liquid at present
The method of chiral analysis.It is therefore desirable to develop, a kind of high sensitivity, precision are good, are suitble to high-volume accurate quantitative analysis electronic cigarette liquid
Middle S- (-)-nicotine and R- (+)-nicotine method.Chiral column-conjunction phase chromatographic tandem mass spectrum has bright in terms of isomer separation
Aobvious advantage, therefore divided by chiral column-conjunction phase chromatographic tandem mass spectrum that many experiments establish nicotine chirality in electronic cigarette liquid
Analysis method, this method are particularly suited for the chiral analysis of nicotine in a large amount of samples.
Summary of the invention
The purpose of the present invention has carried out pre-treating method research to electronic cigarette liquid sample exactly using nicotine as research object,
The analysis method of nicotine optical isomer in series connection chiral column-conjunction phase chromatographic tandem mass spectrography detection electronic cigarette liquid is established, it is real
Show to nicotine optical antipode S- (-)-nicotine in electronic cigarette liquid and R- (+)-nicotine Accurate Determining.
The purpose of the present invention is achieved through the following technical solutions: electronic cigarette liquid sample is passed through sodium hydroxide solution
After mixing, using methyl tertiary butyl ether(MTBE) and methanol solution extraction, extract liquor uses series connection after Dispersive solid phase extraction purifies
Chiral column-conjunction phase chromatographic tandem analytical reagent composition, using S- (-)-nicotine in areas of peak normalization method quantitative detection electronic cigarette liquid
With R- (+)-nicotine ratio.Specific step is as follows:
1. the preparation of standard solution: weighing S- (-)-nicotine standard product of about 100.0 mg, dilute constant volume with methanol solution
Into 50 mL brown volumetric flasks, it is configured to S- (-)-nicotine standard stock solution that concentration is about 2.0 mg/mL；Weigh about 50.0
The R- (+) of mg-nicotine standard product, with methanol solution dilution constant volume into 50 mL brown volumetric flasks, being configured to concentration is about 1.0
The R- (+) of mg/mL-nicotine standard stock solution；It is dilute using S- (-)-nicotine standard stock solution and R- (+)-nicotine standard stock solution
It releases preparation S- (-)-nicotine and R- (+)-nicotinic density is respectively the mixed standard solution of 100 μ g/mL and 80 μ g/mL.
2. the mixing of electronic cigarette liquid sample: electronic cigarette liquid sample being vibrated with 200 r/min and is mixed.
3. the extraction of electronic cigarette liquid sample: weighing 0.3 g sample and have in plug centrifuge tube in 15 mL, 2.0 mL 5% are added
Sodium hydroxide solution, be vortexed 1 min mix after stand 10 min infiltration sample.Take 10 mL methyl tertiary butyl ether(MTBE)s and methanol
(90:10, V/V) solution into centrifuge tube, and on vortex mixer with 4000 rpm velocity fluctuation, 30 min.
4. the purification of extract liquor: supernatant (it is anhydrous to include 150 mg in 2 mL purification centrifuge tube after taking 1.5 mL to extract
Magnesium sulfate, 25 mg PSA adsorbents, 7.5 mg GCB adsorbents are referred to as Dispersive solid phase extraction material), it is mixed in vortex
2 min are vibrated with 4000 rpm on device, are centrifuged 1 min with 10000 rpm.Supernatant is taken to cross 0.45 μm of organic phase filter membrane laggard
Liquid phase analysis.
5. chiral column-conjunction phase chromatographic tandem mass spectrography condition of connecting: analytical column 1 is Trefoil CEL1 column (column length 150
Mm, 3.0 mm of internal diameter, 2.5 μm of stationary phase partial size), analytical column 2 is Chiralcel OD-H liquid-phase chromatographic column (column length 250
Mm, 4.6 mm of internal diameter, 5 μm of stationary phase partial size)；Mobile phase A are as follows: CO2, Mobile phase B: the methanol containing 0.05% isopropylamine；Stream
Speed is 1.1 mL/min；Condition of gradient elution are as follows: 0.0 min, 97% A；0.5 min, 97% A；8.0 min, 92% A；10.0
Min, 92% A；10.2 min, 97% A；12.0 min, 97% A.40 DEG C of column temperature；Sample introduction room temperature: 10 DEG C；Sampling volume 2
μL；Back pressure: 1600 psi；ISM compensation flow path is mutually the methanol containing 0.1% formic acid, and flow velocity is 0.3 mL/min.When analysis
Between amount to 12 min.Mass Spectrometry Conditions: ion source: electrospray ionization source, scanning mode are positive ion scan, ion source temperature 300
DEG C, electron spray voltage is 5000 V, and atomization gas pressure is 40 psi；Detection mode: multiple-reaction monitoring (MRM)；MRM parameter is seen below
Table.By quantitative S- (-)-nicotine being normalized to peak area and R- (+)-nicotine accounts for the ratio of total nicotine.
The present invention provides a kind of chiral analysis of nicotine in electronic cigarette liquid to close phase chromatographic tandem mass spectrography, has following excellent
Good effect: can reduce pollution of the sample liquid to chromatographic column, close phase chromatographic tandem mass spectrography detection method high sensitivity, specificity
It is good, it can avoid false positive, analysis time is short, is able to achieve to S- (-)-nicotine and R- (+)-nicotine baseline separation, R- (+)-cigarette
The detection limit (LOD) of alkali is 0.04%, can satisfy the chiral analysis of nicotine in high-volume electronic cigarette liquid sample.
Detailed description of the invention
Fig. 1 is the chromatogram of mixed standard solution,
Fig. 2 is the chromatogram of electronic cigarette liquid sample.
Specific embodiment
The present invention is further described by following specific embodiments, but does not limit the present invention.
1. instrument and reagent
ACQUITY UPC2 ultra high efficiency closes chromatography (Waters, US), 6410B triplex tandem level four bars mass spectrum
Instrument (Agilent company, the U.S.), AE163 electronic balance (sensibility reciprocal: 0.0001 g, Mettler company, Switzerland), high speed disintegrator
(Wuhan Yin Cai Science and Technology Ltd.), U.S.'s ColeparmerVotex-Genie vortex oscillator, German SIGMA 3-30K- high
The desk-top frozen type centrifuge of speed.Methyl tertiary butyl ether(MTBE) (chromatographically pure), sodium hydroxide (analysis is pure), formic acid (chromatographically pure), methanol
(chromatographically pure), S- (-)-nicotine standard product (CAS:54-11-5), R- (+)-nicotine standard product (CAS:25162-00-9).
2. the preparation of standard solution
S- (-)-nicotine standard product for weighing about 100.0 mg dilute constant volume to 50 mL brown volumetric flasks with methanol solution
In, it is configured to S- (-)-nicotine standard stock solution that concentration is about 2.0 mg/mL；Weigh R- (+)-nicotine mark of about 50.0 mg
Quasi- product are configured to R- (+)-cigarette that concentration is about 1.0 mg/mL with methanol solution dilution constant volume into 50 mL brown volumetric flasks
Alkali standard reserving solution；S- (-)-nicotine is prepared using S- (-)-nicotine standard stock solution and R- (+)-nicotine standard stock solution dilution
It is respectively the mixed standard solution of 100 μ g/mL and 80 μ g/mL with R- (+)-nicotinic density.
3. the mixing of electronic cigarette liquid sample: electronic cigarette liquid sample being vibrated with 200 r/min and is mixed.
4. the extraction of electronic cigarette liquid sample: weighing the sample that 0.3 g has been crushed and have in plug centrifuge tube in 15mL, be added
The sodium hydroxide solution of 2.0mL 5%, vortex 1min stand 10 min infiltration sample after mixing.Take 10 mL methyl tertiary butyl ether(MTBE)s
With methanol (90:10, V/V) solution into centrifuge tube, and on vortex mixer with 4000 rpm velocity fluctuation, 30 min.
5. the purification of extract liquor: 1.5 mL supernatants being taken (to include 150 mg anhydrous slufuric acids in 2 mL purification centrifuge tube
Magnesium, 25 mg PSA adsorbents, 7.5 mg GCB adsorbents), on vortex mixer with 4000 rpm vibrate 2 min, with
10000 rpm are centrifuged 1min.Supernatant is taken to cross 0.45 μm of laggard liquid phase analysis of organic phase filter membrane.
6. chiral column-conjunction phase chromatographic tandem mass spectrography condition of connecting: analytical column 1 is Trefoil CEL1 column (column length 150
Mm, 3.0 mm of internal diameter, 2.5 μm of stationary phase partial size), analytical column 2 is Chiralcel OD-H liquid-phase chromatographic column (column length 250
Mm, 4.6 mm of internal diameter, 5 μm of stationary phase partial size)；Mobile phase A are as follows: CO2, Mobile phase B: the methanol containing 0.05% isopropylamine；Stream
Speed is 1.1 mL/min；Condition of gradient elution are as follows: 0.0 min, 97% A；0.5 min, 97% A；8.0 min, 92% A；10.0
Min, 92% A；10.2 min, 97% A；12.0 min, 97% A.40 DEG C of column temperature；Sample introduction room temperature: 10 DEG C；Sampling volume 2
μL；Back pressure: 1600 psi；ISM compensation flow path is mutually the methanol containing 0.1% formic acid, and flow velocity is 0.3 mL/min.When analysis
Between amount to 12 min.Mass Spectrometry Conditions: ion source: electrospray ionization source, scanning mode are positive ion scan, ion source temperature 300
DEG C, electron spray voltage is 5000 V, and atomization gas pressure is 40 psi；Detection mode: multiple-reaction monitoring (MRM)；MRM parameter is seen below
Table.By quantitative S- (-)-nicotine being normalized to peak area and R- (+)-nicotine accounts for the ratio of total nicotine.
7. R- (+)-nicotine detection limit
The chiral composition of nicotine usually accounts for the percentage of total nicotine with R- (+)-nicotine to indicate.To assess R- (+)-nicotine
Detection limit, the standard solution of R- (+)-nicotine is added in the method for the present invention in S- (-)-nicotine standard solution.The result shows that
R- (+)-nicotine response signal can be observed in S- (-)-nicotine standard solution, normalizing is carried out to quota ion peak area
After change, R- (+)-nicotine ratio is 0.04%(peak area relative to total nicotine peak area in S- (-)-nicotine standard solution),
In this, as this method R- (+)-nicotine detection limit.
8. the chiral analysis example of nicotine in electronic cigarette liquid sample
The electronic cigarette liquid sample handled according to above-mentioned steps is carried out to close the mass spectral analysis of phase chromatographic tandem；Using electronic cigarette liquid
MRM ion carries out qualitative analysis, and quantitative S- (-)-nicotine is normalized to peak area and R- (+)-nicotine accounts for the ratio of total nicotine
Example.
10 electronic cigarette liquid samples are analyzed using this method, the results are shown in Table 1.
9. the precision of analysis method
It takes same electronic cigarette liquid sample in a few days and be in the daytime measured in parallel for 5 times, has investigated the precision of the method for the present invention,
It the results are shown in Table 2 and table 3.The result shows that R- (+)-nicotine in a few days and in the daytime variation lines of measurement result in electronic cigarette liquid sample
Number is respectively 9.19% and 7.92%, and precision is preferable.
Above-mentioned 10 electronic cigarette liquid samples are detected using the method in specific embodiment.Detect obtained color
Spectrogram is as depicted in figs. 1 and 2.
Claims (1)
1. the chiral analysis of nicotine closes phase chromatographic tandem mass spectrography in a kind of electronic cigarette liquid, it is characterised in that: by electronic cigarette liquid sample
Product are after sodium hydroxide solution mixes, and using methyl tertiary butyl ether(MTBE) and methanol solution extraction, extract liquor is through matrix dispersed solid phase
After extracting and purifying, using chiral column-conjunction phase chromatographic tandem analytical reagent composition, using areas of peak normalization method quantitative detection electronic cigarette
S- (-)-nicotine and R- (+)-nicotine ratio in liquid, the specific steps are as follows:
1) preparation of standard solution: weighing S- (-)-nicotine standard product of about 100.0 mg, is arrived with methanol solution dilution constant volume
In 50 mL brown volumetric flasks, it is configured to S- (-)-nicotine standard stock solution that concentration is about 2.0 mg/mL；Weigh about 50.0 mg
R- (+)-nicotine standard product, with methanol solution dilution constant volume into 50 mL brown volumetric flasks, being configured to concentration is about 1.0
The R- (+) of mg/mL-nicotine standard stock solution；It is dilute using S- (-)-nicotine standard stock solution and R- (+)-nicotine standard stock solution
It releases, prepares S- (-)-nicotine and R- (+)-nicotinic density is respectively the mixed standard solution of 100 μ g/mL and 80 μ g/mL；
2) mixing of electronic cigarette liquid sample: electronic cigarette liquid sample is vibrated with 200 r/min and is mixed；
3) it the extraction of electronic cigarette liquid sample: weighs 0.3 g sample and has in plug centrifuge tube in 15 mL, be added 2.0 mL's 5%
Sodium hydroxide solution, 1 min that is vortexed stand 10 min infiltration sample, 10 mL methyl tertiary butyl ether(MTBE)s/methanol solution are taken to arrive after mixing
In above-mentioned tool plug centrifuge tube, and on vortex mixer with 4000 rpm velocity fluctuation, 30 min；Methyl tertiary butyl ether(MTBE) and methanol
Volume ratio 90:10
4) purification of extract liquor: take 1.5 mL extraction supernatant in the purification containing Dispersive solid phase extraction material in 2 mL
In centrifuge tube, in vibrating 2 min on vortex mixer with 4000 rpm, it is centrifuged 1 min with 10000 rpm, takes supernatant mistake
The laggard conjunction phase chromatographic tandem mass spectral analysis of 0.45 μm of organic phase filter membrane；The Dispersive solid phase extraction material contains: 150 mg
Anhydrous magnesium sulfate, 25 mg PSA adsorbents, 7.5 mg GCB adsorbents；
5) series connection chiral column-conjunction phase chromatographic tandem mass spectrography condition: analytical column 1 is Trefoil CEL1 column, 150 mm of column length
, 3.0 mm of internal diameter, 2.5 μm of stationary phase partial size, analytical column 2 be Chiralcel OD-H liquid-phase chromatographic column, 250 mm of column length,
4.6 mm of internal diameter, 5 μm of stationary phase partial size；Mobile phase A are as follows: CO2, Mobile phase B: the methanol containing 0.05% isopropylamine；Flow velocity is
1.1 mL/min；Condition of gradient elution are as follows: 0.0 min, 97% A；0.5 min, 97% A；8.0 min, 92% A；10.0 min,
92% A；10.2 min, 97% A；12.0 min, 97% A；40 DEG C of column temperature；Sample introduction room temperature: 10 DEG C；2 μ L of sampling volume；
Back pressure: 1600 psi；ISM compensation flow path is mutually the methanol containing 0.1% formic acid, and flow velocity is 0.3 mL/min；Analysis time is total
Count 12 min；Mass Spectrometry Conditions: ion source: electrospray ionization source, scanning mode are positive ion scan, and ion source temperature is 300 DEG C, electricity
Spray voltage is 5000 V, and atomization gas pressure is 40 psi；Detection mode: multiple-reaction monitoring；By carrying out normalizing to peak area
Change quantitative S- (-)-nicotine and R- (+)-nicotine accounts for the ratio of total nicotine.
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| CN107367555B (en) * | 2017-06-29 | 2019-09-06 | 国家烟草质量监督检验中心 | Nicotine and chiral resolution measuring method while nornicotine in a kind of tobacco juice for electronic smoke |
| CN107247107A (en) * | 2017-08-15 | 2017-10-13 | 国家烟草质量监督检验中心 | A kind of method for closing nornicotine enantiomter content in phase chromatographic tandem mass spectrometric determination cigarette shreds |
| CN107228914A (en) * | 2017-08-15 | 2017-10-03 | 国家烟草质量监督检验中心 | A kind of method for closing nornicotine enantiomter content in phase chromatographic tandem mass spectrometric determination smoke-free tobacco product |
| CN107478746A (en) * | 2017-08-15 | 2017-12-15 | 国家烟草质量监督检验中心 | The chiral analysis of nicotine and nornicotine close phase chromatographic tandem mass spectrography in a kind of electronic cigarette liquid |
| CN107505411A (en) * | 2017-08-15 | 2017-12-22 | 国家烟草质量监督检验中心 | A kind of method for closing nornicotine enantiomter content in phase chromatographic tandem mass spectrometric determination tobacco juice for electronic smoke |
| CN107478745A (en) * | 2017-08-15 | 2017-12-15 | 国家烟草质量监督检验中心 | Nicotine and nornicotine chiral analysis close phase chromatographic tandem mass spectrography in a kind of smoke-free tobacco product |
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| CN103698458B (en) * | 2013-12-26 | 2015-03-11 | 国家烟草质量监督检验中心 | Method for measuring main carbonyl compounds in main stream smoke of cigarette through ultra high performance convergence chromatography |
| CN104133023B (en) * | 2014-08-25 | 2015-09-02 | 国家烟草质量监督检验中心 | A kind of utilization closes the analytical approach that phase chromatogram detects tralomethrin and decis in tobacco simultaneously |
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