CN107228914A - A kind of method for closing nornicotine enantiomter content in phase chromatographic tandem mass spectrometric determination smoke-free tobacco product - Google Patents

A kind of method for closing nornicotine enantiomter content in phase chromatographic tandem mass spectrometric determination smoke-free tobacco product Download PDF

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Publication number
CN107228914A
CN107228914A CN201710697590.1A CN201710697590A CN107228914A CN 107228914 A CN107228914 A CN 107228914A CN 201710697590 A CN201710697590 A CN 201710697590A CN 107228914 A CN107228914 A CN 107228914A
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smoke
nornicotine
sample
free tobacco
nornicotines
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陈欢
韩书磊
付亚宁
刘彤
侯宏卫
胡清源
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NATIONAL TOBACCO QUALITY SUPERVISION TESTING CENTER
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NATIONAL TOBACCO QUALITY SUPERVISION TESTING CENTER
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    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N30/00Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
    • G01N30/02Column chromatography
    • G01N30/04Preparation or injection of sample to be analysed
    • G01N30/06Preparation
    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N30/00Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
    • G01N30/02Column chromatography
    • G01N30/88Integrated analysis systems specially adapted therefor, not covered by a single one of the groups G01N30/04 - G01N30/86
    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N30/00Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
    • G01N30/02Column chromatography
    • G01N30/88Integrated analysis systems specially adapted therefor, not covered by a single one of the groups G01N30/04 - G01N30/86
    • G01N2030/8809Integrated analysis systems specially adapted therefor, not covered by a single one of the groups G01N30/04 - G01N30/86 analysis specially adapted for the sample

Abstract

The invention discloses a kind of method for closing nornicotine enantiomter content in phase chromatographic tandem mass spectrometric determination smoke-free tobacco product.It is characterized in that:By smoke-free tobacco product sample drying, crush and sieving, sample is after sodium hydroxide solution infiltrates, extracted using dichloromethane, after extract is purified through Dispersive solid phase extraction, phase chromatographic tandem analytical reagent composition is closed using two chiral column series connection, the ratio of S nornicotines and R nornicotines in smoke-free tobacco product is quantitatively detected using areas of peak normalization method.The detection method that this method is provided, sample extraction purification method is simply efficient, pollution of the sample liquid to chromatographic column can be reduced, close the sensitivity of phase chromatographic tandem mass spectrography detection method high, specificity is good, false positive can be excluded, analysis time is short, disclosure satisfy that the chiral analysis of nornicotine in high-volume smoke-free tobacco product sample.

Description

One kind closes phase chromatogram-tandem mass spectrometry and determines nornicotine pair in smoke-free tobacco product Reflect the method for content of isomer
Technical field
The invention belongs to physico-chemical analysis technical field, and in particular to one kind closes phase chromatogram-tandem mass spectrometry and determines smokeless The method of nornicotine enantiomter content in tobacco product.
Background technology
Nornicotine is one of main alkaloid in smoke-free tobacco product, has important shadow to smoke-free tobacco product quality Ring, and be tobacco-specific nitrosamine --- nitrosonornicotine(NNN)Precursor substance.Nornicotine molecule contains in a chirality The heart, so nornicotine has two enantiomers:S- (-)-nornicotine(Abbreviation S- nornicotines)With R- (+)-nornicotine(Cigarette drops in abbreviation R- Alkali).According to the characteristic of enantiomter, two mapping enantiomers of nornicotine may have entirely different metabolic mechanism and life Manage characteristic.Therefore, it is necessary to which the enantiomter content to nornicotine in smoke-free tobacco product carries out analysis measure.
At present, the assay method of document report nornicotine enantiomter mainly has gas chromatography-mass spectrometry(GC- MS, Beitr ge Zur Tabakforschung. 2013;25(7):649-659. Chirality. 1999;11(1):82- 84.), multidimensional gas chromatographic-MS(MDGC-MS, J. Chromatogr. B. 2008;865(1):13-17.), hair Cons electrophoresis method(CE, Electrophoresis. 2009;30(2):349–356.)Deng, still, GC-MS and MDGC-MS needs Perform the derivatization, waste time and energy in pretreatment process, CE is qualitative using only retention time progress, and qualitative ability is relatively poor, Easily there are false positive results.It is therefore desirable to develop, a kind of sensitivity is high, precision is good, it is smokeless to be adapted to high-volume accurate quantitative analysis The method of S- nornicotines and R- nornicotines in gas tobacco product.
The content of the invention
The purpose of the present invention is based on above-mentioned technical deficiency, establishes a kind of phase chromatogram-tandem mass spectrometry that closes and determines nothing The method of nornicotine enantiomter content in flue gas tobacco product.This method does not need derivatization mistake in pretreatment process Journey, realizes the baseline separation of S- nornicotines and R- nornicotines, and carry out qualitative using second order mses and quantify, it is to avoid occur false Positive findings, so, this method has the advantages that easy to operate, sensitivity is high, accurately set.
The purpose of the present invention is achieved through the following technical solutions:
By smoke-free tobacco product sample drying, crush and sieving, sample is after sodium hydroxide solution infiltrates, using dichloromethane Alkane is extracted, after extract is purified through Dispersive solid phase extraction, using series connection chiral column-conjunction phase chromatogram-tandem mass spectrometry analysis, The ratio of S- nornicotines and R- nornicotines in smoke-free tobacco product is quantitatively detected using areas of peak normalization method.
Comprise the following steps that:
1. the preparation of standard liquid
About 100.0 mg S- (-)-nornicotine standard items are weighed, constant volume is diluted into 50 mL brown volumetric flasks with methanol solution, It is configured to S- (-)-nornicotine standard reserving solution that concentration is about 2.0 mg/mL;Weigh about 100.0 mg R- (+)-nornicotine Standard items, constant volume is diluted into 50 mL brown volumetric flasks with methanol solution, be configured to R- (+) that concentration is about 2.0 mg/mL- Nornicotine standard reserving solution;S- is prepared using S- (-)-nornicotine standard reserving solution and R- (+)-nornicotine standard reserving solution dilution (-)-nornicotine and R- (+)-nornicotine concentration are respectively 100 μ g/mL and 100 μ g/mL mixed standard solution
2. the mixing of smoke-free tobacco product sample
Smoke-free tobacco product sample is placed in 40 DEG C of baking ovens, smoke-free tobacco product is taken out after 1 hour, mistake after crushing 0.45 mm pore size standard screen.
3. the extraction of smoke-free tobacco product sample
N-hexane, methyl tertiary butyl ether(MTBE), ethyl acetate, dichloromethane, five kinds of solvents of chloroform are selected to carry out extraction efficiency Compare.As a result find, dichloromethane takes second place to the extraction efficiency highest of nornicotine, methyl tertiary butyl ether(MTBE) and ethyl acetate, just oneself The extraction efficiency of alkane and chloroform is worst, therefore selection dichloromethane is final extractant.
The extraction step of optimization is:
Sample that 0.3 g crushed is weighed in 15 mL tool plug centrifuge tubes, 2.0 mL 5% sodium hydroxide solution is added(Quality Than), 10 min infiltration samples are stood after the 1 min mixings that are vortexed, 10 mL dichloromethane are taken into centrifuge tube, and in vortex mixing With the min of 4000 rpm velocity fluctuations 30 on device.
4. the purification of extract
1.5 mL supernatants are taken in 2 mL purification centrifuge tubes(Include 150 mg anhydrous magnesium sulfates, 50mg PSA adsorbents, 25 Mg GCB adsorbents, are referred to as Dispersive solid phase extraction material), on vortex mixer with 4000 rpm vibrate 2 min, with 10000 rpm centrifuge 1 min.Supernatant is taken to cross 0.45 μm of laggard liquid phase analysis of organic phase filter membrane.
5. chiral column-conjunction phase chromatogram-tandem mass spectrometry condition of connecting
Analytical column 1 is Trefoil CEL1 posts(The mm of column length 150, the mm of internal diameter 3.0,2.5 μm of stationary phase particle diameter), analytical column 2 be Chiralcel OD-H liquid-phase chromatographic columns (mm of column length 250, the mm of internal diameter 4.6,5 μm of stationary phase particle diameter);Mobile phase A For:CO2, Mobile phase B:Methanol containing 0.05% isopropylamine;Flow velocity is 1.0 mL/min;Condition of gradient elution is:0.0 min, 97% A;0.5 min, 97% A;8.0 min, 92% A;12.0 min, 92% A;30.0 min, 90% A.40 DEG C of column temperature;Enter Specimen chamber temperature:10 ℃;The μ L of sampling volume 2;Back pressure:1600 psi;ISM compensation flow path is mutually the first containing 0.1% formic acid Alcohol, flow velocity is 0.3 mL/min.Analysis time amounts to 30 min.Mass Spectrometry Conditions:Ion gun:Electrospray ionization source, scan mode is just Ion scan, ion source temperature is 300 DEG C, and electron spray voltage is 5000 V, and atomization gas pressure is 40 psi;Detection mode:It is many Reaction monitoring(MRM);MRM parameters see the table below 1.Accounted for always by peak area being normalized quantitative S- nornicotines and R- nornicotines The ratio of nornicotine.
6. detection limit and quantitative limit
With optimal conditions, according to object signal to noise ratio be 3 when corresponding concentration as detection limit, be according to object signal to noise ratio Corresponding concentration is used as detection limit when 10.The detection limit and quantitative limit of S- nornicotines are respectively 0.12 μ g/g and 0.40 μ g/g, The detection limit and quantitative limit of R- nornicotines are respectively 0.12 μ g/g and 0.40 μ g/g.
7. precision
Take same smoke-free tobacco product sample to carry out 5 times in a few days and parallel determination in the daytime, investigate the precision of the inventive method Degree, the results are shown in Table 2 and table 3.As a result show, the in a few days and in the daytime measurement result of S- nornicotines in smoke-free tobacco product sample The coefficient of variation is respectively 1.08% and 2.45%, and precision is preferable.
Phase chromatographic tandem mass spectrography, tool are closed the invention provides a kind of chiral analysis of nornicotine in smoke-free tobacco product There are following excellent results:1. determined first using conjunction phase chromatogram-tandem mass spectrometry detection method in smoke-free tobacco product and drop cigarette Alkali enantiomter content, this method is compared with the method that document report determines nornicotine enantiomter content, with sensitive Degree is high, the good advantage of specificity, can avoid false positive results, and separating degree is good, can realize to S- nornicotines and R- nornicotines Baseline separation;2. by the optimization of extractant, using dichloromethane as extractant, extraction efficiency is optimal;3. extraction is passed through Take the purification of liquid, it is possible to decrease pollution of the sample liquid to chromatographic column;4. analysis time is short, disclosure satisfy that high-volume smokeless tobacco system The chiral analysis of nornicotine in product.
Brief description of the drawings
Fig. 1 is extraction efficiency schematic diagram of the different extractants to target compound.
Fig. 2 is the chromatogram of mixed standard solution.
Fig. 3 is the chromatogram of typical smoke-free tobacco product sample.
Embodiment
The present invention is further described by specific examples below, but does not limit the present invention.
Embodiment 1:
1. instrument and reagent
ACQUITY UPC2 ultra high efficiencies close chromatography(Waters, US), 6410B triplex tandem level Four bar mass spectrographs(It is beautiful Agilent companies of state), AE163 electronic balances(Sensibility reciprocal:0.0001 g, Mettler companies of Switzerland), high speed disintegrator(Wuhan silver Color Science and Technology Ltd.), U.S.'s ColeparmerVotex-Genie turbula shakers, German SIGMA 3-30K- high speed desktops Frozen type centrifuge.Dichloromethane(Chromatographically pure), sodium hydroxide(Analysis is pure), formic acid(Chromatographically pure), methanol(Chromatographically pure), S- drops Nicotine standard product, R- nornicotine standard items.
2. sample pre-treatments
(1)The mixing of smoke-free tobacco product sample:Smoke-free tobacco product sample is placed in 40 DEG C of baking ovens, will after 1 hour Smoke-free tobacco product is taken out, and 0.45 mm pore size standard screen is crossed after crushing.
(2)The extraction of smoke-free tobacco product sample:Sample that 0.3 g crushed is weighed in 15mL tool plug centrifuge tubes, 2.0mL 5% sodium hydroxide solution is added, vortex 1min stands 10 min infiltration samples after mixing.Take 10 mL dichloromethane Into centrifuge tube, and on vortex mixer with the min of 4000 rpm velocity fluctuations 30.
(3)The purification of extract:1.5 mL supernatants are taken in 2 mL purification centrifuge tubes(Include 150 mg anhydrous slufuric acids Magnesium, 50 mg PSA adsorbents, 25 mg GCB adsorbents), in vibrating 2 min on vortex mixer with 4000 rpm, with 10000 Rpm centrifuges 1min.Supernatant is taken to cross 0.45 μm of laggard liquid phase analysis of organic phase filter membrane.
3. the preparation of standard liquid
About 100.0 mg S- (-)-nornicotine standard items are weighed, constant volume is diluted into 50 mL brown volumetric flasks with methanol solution, It is configured to S- (-)-nornicotine standard reserving solution that concentration is about 2.0 mg/mL;Weigh about 100.0 mg R- (+)-nornicotine Standard items, constant volume is diluted into 50 mL brown volumetric flasks with methanol solution, be configured to R- (+) that concentration is about 2.0 mg/mL- Nornicotine standard reserving solution;S- is prepared using S- (-)-nornicotine standard reserving solution and R- (+)-nornicotine standard reserving solution dilution (-)-nornicotine and R- (+)-nornicotine concentration are respectively 100 μ g/mL and 100 μ g/mL mixed standard solution
4. instrumental conditions
Analytical column 1 is Trefoil CEL1 posts(The mm of column length 150, the mm of internal diameter 3.0,2.5 μm of stationary phase particle diameter), analytical column 2 be Chiralcel OD-H liquid-phase chromatographic columns (mm of column length 250, the mm of internal diameter 4.6,5 μm of stationary phase particle diameter);Mobile phase A For:CO2, Mobile phase B:Methanol containing 0.05% isopropylamine;Flow velocity is 1.0 mL/min;Condition of gradient elution is:0.0 min, 97% A;0.5 min, 97% A;8.0 min, 92% A;12.0 min, 92% A;30.0 min, 90% A.40 DEG C of column temperature;Enter Specimen chamber temperature:10 ℃;The μ L of sampling volume 2;Back pressure:1600 psi;ISM compensation flow path is mutually the first containing 0.1% formic acid Alcohol, flow velocity is 0.3 mL/min.Analysis time amounts to 30 min.Mass Spectrometry Conditions:Ion gun:Electrospray ionization source, scan mode is just Ion scan, ion source temperature is 300 DEG C, and electron spray voltage is 5000 V, and atomization gas pressure is 40 psi;Detection mode:It is many Reaction monitoring(MRM);MRM parameters are shown in Table 1.
Quantitative S- nornicotines are normalized to peak area and R- nornicotines account for the ratio of total nornicotine.
According to said determination method, 5 kinds of smoke-free tobacco product samples are selected, the ratio for measuring S- nornicotines is respectively 61.84%th, 67.28%, 65.84%, 62.26% and 67.35%.

Claims (5)

1. a kind of close the method that phase chromatogram-tandem mass spectrometry determines nornicotine enantiomter content in smoke-free tobacco product, It is characterized in that:By smoke-free tobacco product sample drying, crush and sieving, sample is adopted after sodium hydroxide solution infiltrates Extracted with dichloromethane, after extract is purified through Dispersive solid phase extraction, use chiral column-conjunction phase chromatogram-tandem mass spectrum point Analysis, the ratio of S- nornicotines and R- nornicotines in smoke-free tobacco product is quantitatively detected using areas of peak normalization method, specific step It is rapid as follows:
(1)The preparation of standard liquid:100.0 mg S- nornicotine standard items are weighed, constant volume is diluted to 50 mL with methanol solution In brown volumetric flask, the S- nornicotine standard reserving solutions that concentration is 2.0 mg/mL are configured to;Weigh 100.0 mg R- nornicotines Standard items, constant volume is diluted into 50 mL brown volumetric flasks with methanol solution, is configured to the R- nornicotines that concentration is 2.0 mg/mL Standard reserving solution;S- nornicotines and R- drop cigarettes are prepared using S- nornicotines standard reserving solution and the dilution of R- nornicotines standard reserving solution Alkali concn is respectively 100 μ g/mL and 100 μ g/mL mixed standard solution;
(2)The mixing of smoke-free tobacco product sample:Smoke-free tobacco product sample is placed in 40o, will after 1 hour in C baking ovens Smoke-free tobacco product is taken out, and 0.45 mm pore size standard screen is crossed after crushing;
(3)The extraction of smoke-free tobacco product sample:Sample that 0.3 g crushed is weighed in 15 mL tool plug centrifuge tubes, is added 2.0 mL 5% sodium hydroxide solution, 1 min that is vortexed stands 10 min infiltration samples after mixing;10 mL dichloromethane are taken to arrive In above-mentioned tool plug centrifuge tube, and on vortex mixer with the min of 4000 rpm velocity fluctuations 30;
(4)The purification of extract:1.5 mL are taken to extract 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, 1 min is centrifuged with 10000 rpm, supernatant mistake is taken 0.45 μm of laggard liquid phase analysis of organic phase filter membrane;
(5)Series connection chiral column-conjunction phase chromatographic tandem mass spectrography condition:Analytical column 1 is Trefoil CEL1 posts, the mm of column length 150 , the mm of internal diameter 3.0,2.5 μm of stationary phase particle diameter, analytical column 2 be Chiralcel OD-H liquid-phase chromatographic columns, the mm of column length 250, The mm of internal diameter 4.6,5 μm of stationary phase particle diameter;Mobile phase A is:CO2, Mobile phase B:Methanol containing 0.05% isopropylamine;Flow velocity is 1.0 mL/min;Condition of gradient elution is:0.0 min, 97% A;0.5 min, 97% A;8.0 min, 92% A;12.0 min, 92% A;30.0 min, 90% A;40 DEG C of column temperature;Sample introduction room temperature:10 ℃;The μ L of sampling volume 2;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 amounts to 30 min;Mass spectrum Condition:Ion gun:Electrospray ionization source, scan mode scans for cation, and ion source temperature is 300 DEG C, and electron spray voltage is 5000 V, atomization gas pressure is 40 psi;Detection mode:Multiple-reaction monitoring(MRM);By peak area being normalized quantitative S- drops Nicotine and R- nornicotines account for the ratio of total nornicotine.
It is different that 2. conjunction phase chromatogram-tandem mass spectrometry according to claim 1 determines nornicotine mapping in smoke-free tobacco product The method of structure body content, it is characterised in that:Step(4)Described in Dispersive solid phase extraction material contain:The anhydrous sulphur of 150 mg Sour magnesium, 50 mg PSA adsorbents, 25 mg GCB adsorbents.
CN201710697590.1A 2017-08-15 2017-08-15 A kind of method for closing nornicotine enantiomter content in phase chromatographic tandem mass spectrometric determination smoke-free tobacco product Pending CN107228914A (en)

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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN109470789A (en) * 2018-11-15 2019-03-15 贵州省烟草科学研究院 A kind of chiral analysis method of nornicotine, anabasine and anatabine in tobacco and tobacco product
US10405571B2 (en) 2015-06-26 2019-09-10 Altria Client Services Llc Compositions and methods for producing tobacco plants and products having altered alkaloid levels

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CN106814155A (en) * 2017-03-10 2017-06-09 国家烟草质量监督检验中心 The chiral analysis of nicotine close phase chromatographic tandem mass spectrography in a kind of tomato
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* Cited by examiner, † Cited by third party
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CN109470789A (en) * 2018-11-15 2019-03-15 贵州省烟草科学研究院 A kind of chiral analysis method of nornicotine, anabasine and anatabine in tobacco and tobacco product

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