CN107688062A - A kind of method of trace nicotine in measure tobacco juice for electronic smoke - Google Patents
A kind of method of trace nicotine in measure tobacco juice for electronic smoke Download PDFInfo
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- CN107688062A CN107688062A CN201710730240.0A CN201710730240A CN107688062A CN 107688062 A CN107688062 A CN 107688062A CN 201710730240 A CN201710730240 A CN 201710730240A CN 107688062 A CN107688062 A CN 107688062A
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- nicotine
- tobacco juice
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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
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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
Abstract
The present invention relates to a kind of method for determining trace nicotine in tobacco juice for electronic smoke, belong to physico-chemical analysis technical field.This method comprises the following steps：（1）Using 1% sodium hydrate aqueous solution by the nicotine separate out in tobacco juice for electronic smoke；（2）Liquid liquid oscillation extraction is carried out using methyl tertiary butyl ether(MTBE) as extractant；（3）After being stored at room temperature, upper organic phase is taken to be transferred to progress GC MS/MS analyses, inner mark method ration in chromatography bottle.The average recovery of standard addition of nicotine is 98.5% in the present invention, precision 1.02%, and method detection is limited to 4.80 ng/g, has the advantages that easy to operate, high sensitivity, the rate of recovery and reproducible.
Description
Technical field
The invention belongs to physico-chemical analysis technical field, and in particular to a kind of side for determining trace nicotine in tobacco juice for electronic smoke
Method.
Background technology
Electronic cigarette, also known as electronics nicotine transmission system, the tobacco juice in cigarette bullet can be atomized simultaneously by it by built-in atomizer
Atomization gas is delivered to oral cavity and lung, and often containing the horizontal nicotine of various concentrations in atomization gas.Nicotine be electronic cigarette most
Important physiological activator, and there is potential addiction feature, it is significant to its accurate quantitative analysis.At present, commercially available electronics
It is zero to have major part to mark nicotinic density in smoke product, and the method for determining nicotinic density in tobacco juice for electronic smoke at present is general
Analytical instrument is directly entered after diluting for tobacco juice to be analyzed, such as gas chromatography（Addiction 2014, 109 (3),
500-507；Journal of Analytical Science 2015,31 (4), 494-498.）, liquid chromatography（Addiction 2013, 108
(9), 1671-1679.）It is applied to measure high concentration nicotine Deng, these methods, but test limit is relatively low（Respectively 50
Ng/mL, 3700 ng/g and 30 ng/mL）, and the tobacco juice for electronic smoke that partial nicotinic concentration is labeled as zero may contain trace cigarette
Alkali, it may be not enough to reach requirement using the detection sensitivity of this kind of method.In addition, these methods are generally detected using thermion
Device（TSD）, hydrogen flame ionization detector（FID）, UV-detector（UVD）Deng the selectivity of this kind of detector is not strong, may go out
Existing false positive results.
The content of the invention
The purpose of the present invention is based on above-mentioned technical deficiency, establishes a kind of side for determining trace nicotine in tobacco juice for electronic smoke
Method.This method need not be complicated pretreatment process, there is easy to operate, high sensitivity, the rate of recovery and reproducible.
The purpose of the present invention is achieved through the following technical solutions：
A kind of method of trace nicotine in measure tobacco juice for electronic smoke, it is characterised in that：Using the 1% NaOH aqueous solution by target sample
Secondary alkaloid separate out in product, then liquid-liquid extraction is carried out with methyl tertiary butyl ether(MTBE), entered with gas chromatography tandem mass spectrometry instrument
Row measure, inner mark method ration；Specifically include following steps：
1）The preparation of standard working solution
The nicotine standard working solution with 9 grades of concentration gradients is prepared respectively, using quinoline as internal standard；
2）Sample pre-treatments
Accurately weigh about 0.5-2.0 g tobacco juice for electronic smoke samples in 15 mL plastic centrifuge tubes, then be separately added into inner mark solution,
The 5.0 mL1% NaOH aqueous solution and 5.0 mL methyl tertiary butyl ether(MTBE)s, are placed in turbula shaker after sealing, with 2000
The rpm min of speed scroll mechanical shaking extraction 40, after placement is stored at room temperature 0.5 h, upper organic phase is taken to be transferred to chromatography bottle
Middle progress GC-MS/MS analyses；
3）Gas chromatography tandem mass spectrometry is analyzed
Made testing sample solution and standard working solution are analyzed using gas chromatography tandem mass spectrometry instrument, obtain correlation
Chromatogram；
4）Specification Curve of Increasing and result calculate.
In particular the present invention includes herein below：
The preparation of 1 standard liquid
The preparation of 1.1 inner mark solutions
About 100.0 mg quinoline accurately are weighed in 50 mL brown volumetric flasks, with methyl tertiary butyl ether(MTBE) constant volume, produce internal standard deposit
Liquid.Internal standard storing solution is diluted 50 times with methyl tertiary butyl ether(MTBE), that is, obtains inner mark solution.
The preparation of 1.2 primary standard storing solutions
About 20.0mg nicotine accurately is weighed, is placed in 10 mL brown volumetric flask, is released with methyl tertiary butyl ether(MTBE) and be settled to scale.
The solution should be kept in dark place under the conditions of 4 DEG C~8 DEG C.
1.3 the preparation of secondary standard storing solution
About 0.1 mL one-level nicotine standard storing solutions accurately are pipetted, is placed in 10 mL brown volumetric flask, uses methyl tertiary butyl ether(MTBE)
Dilution is settled to scale.The solution should be kept in dark place under the conditions of 4 DEG C~8 DEG C.
The preparation of 1.4 standard working solutions
10 μ L, 20 μ L, 50 μ L, 100 μ L, 200 μ L, 500 μ L, 1000 μ L, 2000 μ L, 5000 μ are accurately pipetted respectively
L two level nicotine standard storing solution is in 10 different mL brown volumetric flasks, then 50 μ L inner mark solutions of accurate addition respectively, uses
Methyl tertiary butyl ether(MTBE) dilution is settled to scale, that is, obtains the series standard solution of 9 various concentrations.
2 instrumental conditions
The instrumental conditions of methods described are：
Chromatographic column：DB-35MS capillary chromatographic columns, stationary phase：（35%- phenyl）- methyl polysiloxane, specification：30 m ×
0.25 mm × 0.25 μm；
Injector temperature：250 ℃；Sample size：1 μL；Carrier gas：Helium, purity >=99.999%, constant current mode, flow velocity：1.0
mL/min；
Post heating schedule：Splitless injecting samples；Solvent delay：5 min；Heating schedule：80 DEG C of initial temperature, 1 min is kept, with 20
DEG C/min rises to 200 DEG C, then with 50 DEG C/min speed to 300 DEG C, keep 5 min；
Ionization mode：Electron bombardment ionization source（EI）；Ionizing energy：70 eV；Transmission line temperature：280 ℃；Ion source temperature：250
℃；Q2 collision gas：Argon gas, 1.2 mTorr；Scanning of the mass spectrum mode：Multiple-reaction monitoring pattern（MRM）, monitoring parameters such as following table institute
Show：
Nicotine and its interior target retention time and MRM parameters
| Object | Retention time（min） | Quota ion pair | Impact energy（eV） | Qualitative ion pair | Impact energy（eV） |
| Nicotine | 6.670 | 84.0>82.1 | 10 | 84.0>67.1 | 19 |
| Quinoline（Internal standard） | 6.284 | 129.0>78.1 | 19 | 129.0>76.1 | 25 |
3 sample pre-treatments
Accurately weigh about 1 g tobacco juice for electronic smoke sample in 15 mL plastic centrifuge tubes, then be separately added into 25 μ L inner mark solutions,
The 5.0 mL1% NaOH aqueous solution and 5.0 mL methyl tertiary butyl ether(MTBE)s, are placed in turbula shaker after sealing, with 2000
The rpm min of speed scroll mechanical shaking extraction 40.After placement is stored at room temperature 0.5 h, upper organic phase is taken to be transferred to chromatography bottle
Middle progress GC-MS/MS analyses.
4 recovery of standard addition and precision
With 1,2- glycol/propane triol systems（1,2- glycol/propane triols mass ratio is 70:30）For vehicle solution, divide
Not according to basic, normal, high 3 kinds it is horizontal add nicotine standard product, each pitch-based sphere replication 5 times, the average mark-on of nicotine returns
Yield is 98.5%, precision 1.02%.
5 ranges of linearity and detection limit
This research is quantified using internal standard method, using the concentration of target compound as abscissa, the peak face of analyte and internal standard compound
Product for ordinate than establishing standard curve.With optimal conditions, it is contemplated that the concentration range of target compound in tobacco juice for electronic smoke,
Be determined the range of linearity of method, and when being 3 according to object signal to noise ratio corresponding concentration as detection limit, the phase of standard curve
Relation number is 0.998, and method detection is limited to 4.80 ng/g.
In a word, this patent establishes a kind of method for determining trace nicotine in tobacco juice for electronic smoke, and this method uses liquid-liquid extraction
Method, sample pre-treatments are more efficient.And it is alkali lye to use 1%NaOH, by the nicotine separate out in tobacco juice for electronic smoke, and is used
Methyl tertiary butyl ether(MTBE) is that extractant is extracted, and inner mark method ration, the detection limit of this method reaches 4.80 ng/g, than existing
Method literature procedure sensitivity is higher by more than an order of magnitude, and high sensitivity greatly improves.In addition, this method uses gas
For phase chromatogram as analytical instrument, separating capacity is strong, using tandem mass spectrometer as detector, has qualitative and quantitation capabilities strong
Advantage, the appearance of false positive results is avoided to greatest extent.
Brief description of the drawings
Fig. 1 is that standard working solution selects ion flow graph.
Fig. 2 is the MRM impact energy optimum results schematic diagrames of nicotine.
Fig. 3 is quinoline（Internal standard）MRM impact energy optimum results schematic diagrames.
Embodiment
The present invention is further described by specific examples below, but does not limit the present invention.
Embodiment 1：
1st, instrument and reagent
Instrument：Gas chromatography tandem mass spectrometry instrument（The triple level Four bar mass spectrographs of Shimadzu 2010-plus gas chromatographs-TQ8030）；
AE163 electronic balances（Sensibility reciprocal：0.0001 g, Mettler companies of Switzerland）；Talboys digital display multitube vortex mixers.
Reagent consumptive material：Nicotine（TRC）, quinoline（alfa）, methyl tertiary butyl ether(MTBE)（DUKSAN, chromatographically pure）, sodium hydroxide（State
Medicine, analysis are pure）, water used is by Milli-Q systems（Milford, MA, USA）It is made.
2nd, sample pre-treatments
Accurately weigh about 1 g tobacco juice for electronic smoke sample in 15 mL plastic centrifuge tubes, then be separately added into 25 μ L inner mark solutions,
The 5.0 mL1% NaOH aqueous solution and 5.0 mL methyl tertiary butyl ether(MTBE)s, are placed in turbula shaker after sealing, with 2000
The rpm min of speed scroll mechanical shaking extraction 40.After placement is stored at room temperature 0.5 h, upper organic phase is taken to be transferred to chromatography bottle
Middle progress GC-MS/MS analyses.
3rd, instrumental conditions
The instrumental conditions of methods described are：
Chromatographic column：DB-35MS capillary chromatographic columns, stationary phase：（35%- phenyl）- methyl polysiloxane, specification：30 m ×
0.25 mm × 0.25 μm。
Injector temperature：250 ℃；Sample size：1 μL；Carrier gas：Helium（Purity >=99.999%）, constant current mode, flow velocity：
1.0 mL/min。
Post heating schedule：Splitless injecting samples；Solvent delay：5 min；Heating schedule：80 DEG C of initial temperature, keep 1
Min, with 20 DEG C/min speed to 200 DEG C, then with 40 DEG C/min speed to 250 DEG C, keep 5 min.When running total
Between be 13.25 min.
Ionization mode：Electron bombardment ionization source（EI）；Ionizing energy：70 eV；Transmission line temperature：280 ℃；Ion source temperature：
250 ℃；Scan ion range：80~250 amu；Scanning of the mass spectrum mode：Select ion surveillance style（SIM）Scanning, object
And interior target retention time, it is quantitative and it is qualitative selection ion parameters it is as shown in table 1.
According to said determination method, select 5 kinds of nicotinic densities to be labeled as zero tobacco juice for electronic smoke sample, measure its nicotine content point
It is not as shown in the table：
| Sample number into spectrum | 1 | 2 | 3 | 4 | 5 |
| Concentration（ng/g） | < LOD | 6510.0 | < LOD | 25.0 | 211.1 |
Claims (1)
- A kind of 1. method for determining trace nicotine in tobacco juice for electronic smoke, it is characterised in that：Using the 1% NaOH aqueous solution by target Secondary alkaloid separate out in sample, then liquid-liquid extraction is carried out with methyl tertiary butyl ether(MTBE), with gas chromatography tandem mass spectrometry method It is measured, inner mark method ration；Specifically include following steps：1）The preparation of standard working solutionThe nicotine standard working solution with 9 grades of concentration gradients is prepared respectively, using quinoline as internal standard；2）Sample pre-treatmentsAccurately weigh about 0.5-2.0 g tobacco juice for electronic smoke samples in 15 mL plastic centrifuge tubes, then be separately added into inner mark solution, The 5.0 mL1% NaOH aqueous solution and 5.0 mL methyl tertiary butyl ether(MTBE)s, are placed in turbula shaker after sealing, with 2000 The rpm min of speed scroll mechanical shaking extraction 40, after placement is stored at room temperature 0.5 h, upper organic phase is taken to be transferred to chromatography bottle Middle progress GC-MS/MS analyses；3）Gas chromatography tandem mass spectrometry instrument is analyzedMade testing sample solution and standard working solution are analyzed using gas chromatography tandem mass spectrometry instrument, obtain correlation Chromatogram, its instrumental conditions are：Chromatographic column：DB-35MS capillary chromatographic columns, stationary phase：（35%- phenyl）- methyl polysiloxane, specification：30 m × 0.25 mm × 0.25 μm；Injector temperature：250 ℃；Sample size：1 μL；Carrier gas：Helium, purity >=99.999%, constant current mode, flow velocity：1.0 mL/min；Post heating schedule：Splitless injecting samples；Solvent delay：5 min；Heating schedule：80 DEG C of initial temperature, 1 min is kept, with 20 DEG C/min rises to 200 DEG C, then with 50 DEG C/min speed to 300 DEG C, keep 5 min；Ionization mode：Electron bombardment ionization source（EI）；Ionizing energy：70 eV；Transmission line temperature：280 ℃；Ion source temperature：250 ℃；Q2 collision gas：Argon gas, 1.2 mTorr；Scanning of the mass spectrum mode：Multiple-reaction monitoring pattern（MRM）, monitoring parameters such as following table institute Show：Nicotine and its interior target retention time and MRM parameters
Object Retention time（min） Quota ion pair Impact energy（eV） Qualitative ion pair Impact energy（eV） Nicotine 6.670 84.0>82.1 10 84.0>67.1 19 Quinoline（Internal standard） 6.284 129.0>78.1 19 129.0>76.1 25 。
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109651335A (en) * | 2019-02-18 | 2019-04-19 | 湖北和诺生物工程股份有限公司 | A kind of racemization agent and preparation method thereof improving R- nicotine racemization rate |
| CN112326860A (en) * | 2020-10-30 | 2021-02-05 | 淄博高新技术产业开发区生物医药研究院 | Method for simultaneously detecting genotoxic impurities of 1, 4-dichlorobutane and 1-chloro-4-hydroxybutane in bulk drug or preparation |
| CN113917044A (en) * | 2021-11-16 | 2022-01-11 | 云南省烟草农业科学研究院 | Method for quantitatively analyzing 11 kinds of amide alkaloids in tobacco leaves by gas chromatography-tandem mass spectrometry |
| CN114577915A (en) * | 2020-11-30 | 2022-06-03 | 上海烟草集团有限责任公司 | Method for measuring free-state and proton-state nicotine content in tobacco juice |
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109651335A (en) * | 2019-02-18 | 2019-04-19 | 湖北和诺生物工程股份有限公司 | A kind of racemization agent and preparation method thereof improving R- nicotine racemization rate |
| CN112326860A (en) * | 2020-10-30 | 2021-02-05 | 淄博高新技术产业开发区生物医药研究院 | Method for simultaneously detecting genotoxic impurities of 1, 4-dichlorobutane and 1-chloro-4-hydroxybutane in bulk drug or preparation |
| CN112326860B (en) * | 2020-10-30 | 2022-12-09 | 淄博高新技术产业开发区生物医药研究院 | Method for simultaneously detecting genotoxic impurities of 1, 4-dichlorobutane and 1-chloro-4-hydroxybutane in bulk drug or preparation |
| CN114577915A (en) * | 2020-11-30 | 2022-06-03 | 上海烟草集团有限责任公司 | Method for measuring free-state and proton-state nicotine content in tobacco juice |
| CN114577915B (en) * | 2020-11-30 | 2023-10-27 | 上海烟草集团有限责任公司 | Method for measuring free nicotine content and proton nicotine content in smoke liquid |
| CN113917044A (en) * | 2021-11-16 | 2022-01-11 | 云南省烟草农业科学研究院 | Method for quantitatively analyzing 11 kinds of amide alkaloids in tobacco leaves by gas chromatography-tandem mass spectrometry |
| CN113917044B (en) * | 2021-11-16 | 2023-10-20 | 云南省烟草农业科学研究院 | Method for quantitatively preparing 11 kinds of amide alkaloids in tobacco leaves by gas chromatography-tandem mass spectrometry |
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