CN107247107A - A kind of method for closing nornicotine enantiomter content in phase chromatographic tandem mass spectrometric determination cigarette shreds - Google Patents

A kind of method for closing nornicotine enantiomter content in phase chromatographic tandem mass spectrometric determination cigarette shreds Download PDF

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Publication number
CN107247107A
CN107247107A CN201710698782.4A CN201710698782A CN107247107A CN 107247107 A CN107247107 A CN 107247107A CN 201710698782 A CN201710698782 A CN 201710698782A CN 107247107 A CN107247107 A CN 107247107A
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nornicotine
cigarette shreds
sample
nornicotines
phase
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Inventor
韩书磊
陈欢
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

Abstract

The invention discloses a kind of method for closing nornicotine enantiomter content in phase chromatographic tandem mass spectrometric determination cigarette shreds.It is characterized in that:By cigarette shreds 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 cigarette shreds 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 cigarette shreds sample.

Description

One kind closes phase chromatogram-tandem mass spectrometry and determines nornicotine enantiomerism in cigarette shreds The method of body content
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 cigarette cigarette The method of nornicotine enantiomter content in silk.
Background technology
Nornicotine is one of main alkaloid in cigarette shreds, cigarette quality is had a major impact, and be that tobacco is peculiar Nitrosamine --- nitrosonornicotine(NNN)Precursor substance.Nornicotine molecule contains a chiral centre, so nornicotine has Two enantiomers:S- (-)-nornicotine(Abbreviation S- nornicotines)With R- (+)-nornicotine(Abbreviation R- nornicotines).It is different according to mapping The characteristic of structure body, two mapping enantiomers of nornicotine may have entirely different metabolic mechanism and physiological property.Therefore, have The necessary enantiomter content to nornicotine in cigarette shreds 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, be adapted to high-volume accurate quantitative analysis cigarette The method of S- nornicotines and R- nornicotines in pipe tobacco.
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 volume The method of nornicotine enantiomter content in cigarette pipe tobacco.This method does not need derivatization process in pretreatment process, realizes The baseline separation of S- nornicotines and R- nornicotines, and carried out using second order mses qualitative and quantitative, it is to avoid there is false positive knot Really, 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 cigarette shreds sample drying, crush and sieving, sample is extracted after sodium hydroxide solution infiltrates using dichloromethane Take, after extract is purified through Dispersive solid phase extraction, using series connection chiral column-conjunction phase chromatogram-tandem mass spectrometry analysis, use Areas of peak normalization method quantitatively detects the ratio of S- nornicotines and R- nornicotines in cigarette shreds.
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 cigarette shreds sample
Cigarette shreds sample is placed in 40 DEG C of baking ovens, cigarette shreds are taken out after 1 hour, 0.45 mm pore size is crossed after crushing Standard screen.
3. the extraction of cigarette shreds 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 cigarette shreds sample to carry out 5 times in a few days and parallel determination in the daytime, investigate the precision of the inventive method, as a result It is shown in Table 2 and table 3.As a result show, the coefficient of variation difference of the in a few days and in the daytime measurement result of S- nornicotines in cigarette shreds sample For 1.08% and 2.45%, precision is preferable.
Phase chromatographic tandem mass spectrography is closed the invention provides a kind of chiral analysis of nornicotine in cigarette shreds, with following Excellent results:1. nornicotine enantiomter in cigarette shreds is determined using conjunction phase chromatogram-tandem mass spectrometry detection method first Content, this method is high with sensitivity compared with the method that document report determines nornicotine enantiomter content, and specificity is good Advantage, false positive results can be avoided, and separating degree is good, can realize the baseline separation to S- nornicotines and R- nornicotines;2. lead to The optimization of extractant is crossed, using dichloromethane as extractant, extraction efficiency is optimal;3., can by the purification of extract Reduce pollution of the sample liquid to chromatographic column;4. analysis time is short, disclosure satisfy that the hand of nornicotine in high-volume cigarette shreds sample Property analysis.
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 cigarette tobacco 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 cigarette shreds sample:Cigarette shreds sample is placed in 40 DEG C of baking ovens, cigarette shreds are taken after 1 hour Go out, 0.45 mm pore size standard screen is crossed after crushing.
(2)The extraction of cigarette shreds sample:Sample that 0.3 g crushed is weighed in 15mL tool plug centrifuge tubes, is added 2.0mL 5% sodium hydroxide solution, vortex 1min stands 10 min infiltration samples after mixing.Take 10 mL dichloromethane to from In heart pipe, 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 cigarette shreds samples are selected, the ratio for measuring S- nornicotines is respectively 61.84%, 67.28%th, 65.84%, 62.26% and 67.35%.

Claims (2)

1. a kind of close the method that phase chromatogram-tandem mass spectrometry determines nornicotine enantiomter content in cigarette shreds, its feature It is:By cigarette shreds sample drying, crush and sieving, sample is extracted after sodium hydroxide solution infiltrates using dichloromethane Take, after extract is purified through Dispersive solid phase extraction, using chiral column-conjunction phase chromatogram-Tandem Mass Spectrometry Analysis, using peak area Normalization method quantitatively detects the ratio of S- nornicotines and R- nornicotines in cigarette shreds, comprises the following steps that:
(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 cigarette shreds sample:Cigarette shreds sample is placed in 40oIn C baking ovens, cigarette shreds are taken out after 1 hour, 0.45 mm pore size standard screen is crossed after crushing;
(3)The extraction of cigarette shreds sample:Sample that 0.3 g crushed is weighed in 15 mL tool plug centrifuge tubes, 2.0 mL are added 5% sodium hydroxide solution, 1 min that is vortexed stands 10 min infiltration samples after mixing;10 mL dichloromethane are taken to above-mentioned tool plug In 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.
2. a kind of phase chromatogram-tandem mass spectrometry that closes according to claim 1 determines nornicotine enantiomerism in cigarette shreds The method of body content, it is characterised in that:Step(4)Described in Dispersive solid phase extraction material contain:150 mg anhydrous slufuric acids Magnesium, 50 mg PSA adsorbents, 25 mg GCB adsorbents.
CN201710698782.4A 2017-08-15 2017-08-15 A kind of method for closing nornicotine enantiomter content in phase chromatographic tandem mass spectrometric determination cigarette shreds Pending CN107247107A (en)

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN107727784A (en) * 2017-11-07 2018-02-23 上海烟草集团有限责任公司 One grow tobacco and tobacco product in the chiral analysis method of nicotine and nornicotine

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CN106885857A (en) * 2017-03-15 2017-06-23 上海烟草集团有限责任公司 One grow tobacco and flue gas in nicotine chiral isomer analysis method
CN106896175A (en) * 2017-03-10 2017-06-27 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 Ling " for giving up smoking
CN106896174A (en) * 2017-03-10 2017-06-27 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 smoke-free tobacco product
CN106896173A (en) * 2017-03-10 2017-06-27 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 electronic cigarette liquid

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Publication number Priority date Publication date Assignee Title
CN102401816A (en) * 2010-09-09 2012-04-04 上海海帝园艺有限公司 Method for detecting alkaloid in tobacco
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
CN106896175A (en) * 2017-03-10 2017-06-27 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 Ling " for giving up smoking
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CN106885857A (en) * 2017-03-15 2017-06-23 上海烟草集团有限责任公司 One grow tobacco and flue gas in nicotine chiral isomer analysis method

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN107727784A (en) * 2017-11-07 2018-02-23 上海烟草集团有限责任公司 One grow tobacco and tobacco product in the chiral analysis method of nicotine and nornicotine

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