CN106896175A - The chiral analysis of nicotine close phase chromatographic tandem mass spectrography in a kind of Ling " for giving up smoking - Google Patents

The chiral analysis of nicotine close phase chromatographic tandem mass spectrography in a kind of Ling " for giving up smoking Download PDF

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CN106896175A
CN106896175A CN201710142381.0A CN201710142381A CN106896175A CN 106896175 A CN106896175 A CN 106896175A CN 201710142381 A CN201710142381 A CN 201710142381A CN 106896175 A CN106896175 A CN 106896175A
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nicotine
ling
giving
smoking
sample
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CN106896175B (en
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庞永强
费婷
张洪非
姜兴益
罗彦波
吴达
戚大伟
李翔宇
朱风鹏
胡少东
付亚宁
陈欢
韩书磊
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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
    • G01N30/62Detectors specially adapted therefor
    • G01N30/72Mass spectrometers
    • G01N30/7233Mass spectrometers interfaced to liquid or supercritical fluid chromatograph
    • G01N30/724Nebulising, aerosol formation or ionisation
    • G01N30/7266Nebulising, aerosol formation or ionisation by electric field, e.g. electrospray
    • 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
    • G01N2030/062Preparation extracting sample from raw material

Abstract

Chiral analysis the invention discloses nicotine in a kind of Ling " for giving up smoking close phase chromatographic tandem mass spectrography.It is characterized in that:By Ling " for giving up smoking sample drying, crush and sieving, sample is by after sodium hydroxide solution infiltration, using methyl tertiary butyl ether(MTBE) and methanol solution extraction, after extract is purified through Dispersive solid phase extraction, connected using two chiral columns and close phase chromatographic tandem analytical reagent composition, using the ratio of S () nicotine and R (+) nicotine in areas of peak normalization method quantitative determination Ling " for giving up smoking.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 phase chromatographic tandem mass spectrography detection method sensitivity high, specificity is good, false positive can be excluded, analysis time is short, disclosure satisfy that the chiral analysis of nicotine in high-volume Ling " for giving up smoking sample.

Description

The chiral analysis of nicotine close phase chromatographic tandem mass spectrography in a kind of Ling " for giving up smoking
Technical field
The present invention relates to Ling " for giving up smoking chemical constituents determination method, and in particular to the chiral analysis of nicotine are closed in a kind of Ling " for giving up smoking Phase chromatographic tandem mass spectrography.
Background technology
Nicotine, is also nicotine, is a kind of alkaloid being present in plant of Solanaceae, is also the important component of tobacco.Cigarette Base molecule contains 2 carbon atoms on a chiral centre, i.e. nafoxidine ring, so nicotine has two enantiomers:S-(-)- Nicotine and R- (+)-nicotine.Two enantiomers of nicotine have entirely different content, metabolic mechanism and physiological property.Therefore need to enter Row Ling " for giving up smoking(Ling " for giving up smoking is the traditional fragrance therapy of medicine principle and motherland using traditional Chinese medicine fragrance consciousness regaining anti-inflammatory, choosing Product is lighted by the imitative cigarette type that modern scientific method is refined with more than 30 kinds of rare Chinese herbal medicines, major part containing nicotine into Point)The chiral analysis of middle nicotine.
The current chiral analysis on nicotine, are mainly studied, for example Application No. using gas chromatography 201610663534.1 patent《A kind of chiral analysis method of nicotine in cigarette shreds》, the method pre-treatment step complexity, And detection time reaches 140min, it is impossible to meet the detection of a large amount of samples, the hand of nicotine in Ling " for giving up smoking is not yet related at present Property analysis method.It is therefore desirable to develop that a kind of sensitivity is high, precision is good, it is adapted to S- in high-volume accurate quantitative analysis Ling " for giving up smoking The method of (-)-nicotine and R- (+)-nicotine.Chiral column-conjunction phase chromatographic tandem mass spectrum has significantly in terms of isomer separation Advantage, therefore the chiral column-conjunction phase chromatographic tandem mass spectrometric analysis method of nicotine chirality in Ling " for giving up smoking is established by many experiments, The method is particularly suited for the chiral analysis of nicotine in a large amount of samples.
The content of the invention
The purpose of the present invention has carried out pre-treating method research exactly with nicotine as research object to Ling " for giving up smoking sample, builds The analysis method of nicotine optical isomer in series connection chiral column-conjunction phase chromatographic tandem mass spectrography detection Ling " for giving up smoking is found, has been realized To the Accurate Determining of nicotine optical antipode S- (-)-nicotine and R- (+)-nicotine in Ling " for giving up smoking.
The purpose of the present invention is achieved through the following technical solutions:By Ling " for giving up smoking sample drying, crush and sieving, sample Product are by after sodium hydroxide solution infiltration, using methyl tertiary butyl ether(MTBE) and methanol solution extraction, extract is through matrix dispersed solid phase After extracting and purifying, using series connection chiral column-conjunction phase chromatographic tandem analytical reagent composition, guarded against using areas of peak normalization method quantitative determination The ratio of S- (-)-nicotine and R- (+)-nicotine in cigarette spirit.Comprise the following steps that:
1. the preparation of standard liquid:S- (-)-nicotine standard product of about 100.0 mg are weighed, constant volume to 50 is diluted with methanol solution In mL brown volumetric flasks, S- (-)-nicotine standard storing solution that concentration is about 2.0 mg/mL is configured to;Weigh about 50.0 mg's R- (+)-nicotine standard product, with methanol solution dilution constant volume to 50 mL brown volumetric flasks, is configured to concentration and is about 1.0 mg/ The R- (+) of mL-nicotine standard storing solution;Matched somebody with somebody using S- (-)-nicotine standard storing solution and R- (+)-nicotine standard storing solution dilution S- (-)-nicotine processed and R- (+)-nicotinic density are respectively the mixed standard solution of 100 μ g/mL and 80 μ g/mL.
2. the mixing of Ling " for giving up smoking sample:Ling " for giving up smoking sample is placed in 40 DEG C of baking ovens, is taken out Ling " for giving up smoking after 1 hour, powder 0.45 mm pore size standard screen is crossed after broken.
3. the extraction of Ling " for giving up smoking sample:Sample that 0.3 g crushed is weighed in 15 mL tool plug centrifuge tubes, 2.0 are added The sodium hydroxide solution of mL 5%, 1 min that is vortexed stands 10 min infiltration samples after mixing.Take 10 mL methyl tertiary butyl ether(MTBE)s and Methyl alcohol(90:10, V/V)Solution in centrifuge tube, and on vortex mixer with the min of 4000 rpm velocity fluctuations 30.
4. the purification of extract:Take 1.5 mL supernatants in 2 mL purification centrifuge tube in(Include 150 mg anhydrous slufuric acids Magnesium, 25 mg PSA adsorbents, 7.5 mg GCB adsorbents;It is referred to as Dispersive solid phase extraction material), on vortex mixer 2 min are vibrated with 4000 rpm, 1 min is centrifuged with 10000 rpm.Take supernatant and cross 0.45 μm of laggard conjunction phase of organic phase filter membrane Chromatographic tandem mass spectral analysis.
5. connect chiral column-conjunction phase chromatographic tandem mass spectrography condition:Analytical column 1 is Trefoil CEL1 posts(Column length 150 Mm, the mm of internal diameter 3.0,2.5 μm of fixing phase particle diameter), analytical column 2 is Chiralcel OD-H liquid-phase chromatographic column (column lengths 250 Mm, the mm of internal diameter 4.6,5 μm of fixing phase particle diameter);Mobile phase A is:CO2, Mobile phase B:Methyl alcohol containing 0.05% isopropylamine;Stream Speed is 1.1 mL/min;Condition of gradient elution is: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 ℃;Sampling volume 2 μL;Back pressure:1600 psi;ISM compensation flow path is mutually the methyl alcohol containing 0.1% formic acid, and flow velocity is 0.3 mL/min.During analysis Between amount to 12 min.Mass Spectrometry Conditions:Ion gun:Electrospray ionization source, scan mode is scanned for cation, and ion source temperature is 300 DEG C, electron spray voltage is 5000 V, and atomization gas pressure is 40 psi;Detection mode:Multiple-reaction monitoring(MRM);MRM parameters see below Table.By to peak area being normalized quantitative S- (-)-nicotine and R- (+)-nicotine accounts for the ratio of total nicotine.
Chiral analysis the invention provides nicotine in a kind of Ling " for giving up smoking close phase chromatographic tandem mass spectrography, with following excellent Effect:Pollution of the sample liquid to chromatographic column is reduced, conjunction phase chromatographic tandem mass spectrography detection method sensitivity is high, and specificity is good, can False positive is avoided, analysis time is short, the baseline separation to S- (-)-nicotine and R- (+)-nicotine, the inspection of R- (+)-nicotine can be realized Rising limit(LOD)It is 0.04%, disclosure satisfy that the chiral analysis of nicotine in high-volume Ling " for giving up smoking sample.
Brief description of the drawings
Fig. 1 is the chromatogram of mixed standard solution,
Fig. 2 is the chromatogram of Ling " for giving up smoking sample.
Specific embodiment
The present invention is further described by specific examples below, but does not limit the present invention.
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 vortex oscillators, German SIGMA 3-30K- high speed desktops Frozen type centrifuge.Methyl tertiary butyl ether(MTBE)(Chromatographically pure), NaOH(Analysis is pure), formic acid(Chromatographically pure), methyl alcohol(Chromatogram It is pure), S- (-)-nicotine standard product(CAS:54-11-5), R- (+)-nicotine standard product(CAS:25162-00-9).
2. the preparation of standard liquid
S- (-)-nicotine standard product of about 100.0 mg are weighed, with methanol solution dilution constant volume to 50 mL brown volumetric flasks, is matched somebody with somebody It is made S- (-)-nicotine standard storing solution that concentration is about 2.0 mg/mL;R- (+)-nicotine standard product of about 50.0 mg are weighed, With in methanol solution dilution constant volume to 50 mL brown volumetric flasks, R- (+)-nicotine standard that concentration is about 1.0 mg/mL is configured to Storing solution;S- (-)-nicotine and R- are prepared using S- (-)-nicotine standard storing solution and R- (+)-nicotine standard storing solution dilution (+)-nicotinic density is respectively the mixed standard solution of 100 μ g/mL and 80 μ g/mL.
3. the mixing of Ling " for giving up smoking sample:Ling " for giving up smoking sample is placed in 40 DEG C of baking ovens, is taken out Ling " for giving up smoking after 1 hour, powder 0.45 mm pore size standard screen is crossed after broken.
4. the extraction of Ling " for giving up smoking sample:Sample that 0.3 g crushed is weighed in 15mL tool plug centrifuge tubes, 2.0mL is added 5% sodium hydroxide solution, vortex 1min stands 10 min infiltration samples after mixing.Take 10 mL methyl tertiary butyl ether(MTBE)s and methyl alcohol (90:10, V/V)Solution in centrifuge tube, and on vortex mixer with the min of 4000 rpm velocity fluctuations 30.
5. the purification of extract:Take 1.5 mL supernatants in 2 mL purification centrifuge tube in(Include 150 mg anhydrous slufuric acids 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.Take supernatant and cross 0.45 μm of laggard liquid phase analysis of organic phase filter membrane.
6. connect chiral column-conjunction phase chromatographic tandem mass spectrography condition:Analytical column 1 is Trefoil CEL1 posts(Column length 150 Mm, the mm of internal diameter 3.0,2.5 μm of fixing phase particle diameter), analytical column 2 is Chiralcel OD-H liquid-phase chromatographic column (column lengths 250 Mm, the mm of internal diameter 4.6,5 μm of fixing phase particle diameter);Mobile phase A is:CO2, Mobile phase B:Methyl alcohol containing 0.05% isopropylamine;Stream Speed is 1.1 mL/min;Condition of gradient elution is: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 ℃;Sampling volume 2 μL;Back pressure:1600 psi;ISM compensation flow path is mutually the methyl alcohol containing 0.1% formic acid, and flow velocity is 0.3 mL/min.During analysis Between amount to 12 min.Mass Spectrometry Conditions:Ion gun:Electrospray ionization source, scan mode is scanned for cation, and ion source temperature is 300 DEG C, electron spray voltage is 5000 V, and atomization gas pressure is 40 psi;Detection mode:Multiple-reaction monitoring(MRM);MRM parameters see below Table.By to peak area being normalized quantitative S- (-)-nicotine and R- (+)-nicotine accounts for the ratio of total nicotine.
7. the detection limit of R- (+)-nicotine
The chiral composition of nicotine generally accounts for the percentage of total nicotine to represent with R- (+)-nicotine.It is the inspection of assessment R- (+)-nicotine Rising limit, the inventive method adds the standard liquid of R- (+)-nicotine in the standard liquid of S- (-)-nicotine.Result shows, S- The response signal of R- (+)-nicotine can be observed in the standard liquid of (-)-nicotine, quota ion peak area is normalized Afterwards, the ratio of R- (+)-nicotine is 0.04% in the standard liquid of S- (-)-nicotine(Peak area is relative to total nicotine peak area), with This as this method R- (+)-nicotine detection limit.
8. in Ling " for giving up smoking sample nicotine chiral analysis example
The Ling " for giving up smoking sample that will be processed according to above-mentioned steps carries out closing phase chromatographic tandem mass spectral analysis;Using Ling " for giving up smoking MRM ions Qualitative analysis is carried out, quantitative S- (-)-nicotine is normalized to peak area and R- (+)-nicotine is accounted for the ratio of total nicotine.
6 Ling " for giving up smoking samples are analyzed using the method, the results are shown in Table 1.
9. the precision of analysis method
Taking same Ling " for giving up smoking sample carries out 5 times in a few days and parallel determination in the daytime, has investigated the precision of the inventive method, as a result sees Table 2 and table 3.Result shows, in Ling " for giving up smoking sample R- (+)-nicotine in a few days and in the daytime the coefficient of variation of measurement result is respectively 6.87% and 8.79%, precision is preferable.
Above-mentioned 6 Ling " for giving up smoking samples are detected using the method in specific embodiment.The chromatogram that detection is obtained Figure is as depicted in figs. 1 and 2.

Claims (3)

1. the chiral analysis of nicotine close phase chromatographic tandem mass spectrography in a kind of Ling " for giving up smoking, it is characterised in that:Ling " for giving up smoking sample is done Dry, crushing and sieving, sample, using methyl tertiary butyl ether(MTBE) and methanol solution extraction, are extracted by after sodium hydroxide solution infiltration After liquid is purified through Dispersive solid phase extraction, using chiral column-conjunction phase chromatographic tandem mass spectral analysis, using areas of peak normalization method The ratio of S- (-)-nicotine and R- (+)-nicotine, comprises the following steps that in quantitative determination Ling " for giving up smoking:
1) preparation of standard liquids:S- (-)-nicotine standard product of about 100.0 mg are weighed, diluting constant volume with methanol solution arrives In 50 mL brown volumetric flasks, S- (-)-nicotine standard storing solution that concentration is about 2.0 mg/mL is configured to;Weigh about 50.0 mg R- (+)-nicotine standard product, dilute constant volume in 50 mL brown volumetric flasks with methanol solution, be configured to concentration and be about 1.0 The R- (+) of mg/mL-nicotine standard storing solution;It is dilute using S- (-)-nicotine standard storing solution and R- (+)-nicotine standard storing solution Release preparation 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 Ling " for giving up smoking sample:Ling " for giving up smoking sample is placed in 40oIn C baking ovens, Ling " for giving up smoking is taken out after 1 hour, after crushing Cross 0.45 mm pore size standard screen;
3) extraction of Ling " for giving up smoking 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, take 10 mL methyl tertiary butyl ether(MTBE)s and methyl alcohol Solution in above-mentioned tool plug centrifuge tube, and on vortex mixer with the min of 4000 rpm velocity fluctuations 30;
4) purification of extracts:Take the purification that 1.5 mL extraction supernatants are contained within Dispersive solid phase extraction material in 2 mL In centrifuge tube, in 2 min are vibrated with 4000 rpm on vortex mixer, 1 min is centrifuged with 10000 rpm, takes supernatant mistake 0.45 μm of laggard conjunction phase chromatographic tandem mass spectral 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 fixing 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 fixing phase particle diameter;Mobile phase A is:CO2, Mobile phase B:Methyl alcohol containing 0.05% isopropylamine;Flow velocity is 1.1 mL/min;Condition of gradient elution is: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 ℃;The μ L of sampling volume 2; Back pressure:1600 psi;ISM compensation flow path is mutually the methyl alcohol containing 0.1% formic acid, and flow velocity is 0.3 mL/min, and analysis time is total Count 12 min;Mass Spectrometry Conditions:Ion gun:Electrospray ionization source, scan mode is scanned for cation, 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(MRM);Carried out by peak area Quantitative S- (-)-nicotine of normalization and R- (+)-nicotine account for the ratio of total nicotine.
2. the chiral analysis of nicotine close phase chromatographic tandem mass spectrography in Ling " for giving up smoking according to claim 1, it is characterised in that: Step 3) in methyl tertiary butyl ether(MTBE)/methanol solution volume ratio 90:10
3. the chiral analysis of nicotine close phase chromatographic tandem mass spectrography in Ling " for giving up smoking according to claim 1, it is characterised in that: Step 4) described in Dispersive solid phase extraction material contain:150 mg anhydrous magnesium sulfates, 25 mg PSA adsorbents, 7.5 mg GCB adsorbents.
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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
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

Citations (8)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103499668A (en) * 2013-09-30 2014-01-08 国家烟草质量监督检验中心 UPC<2> (ultra performance convergence chromatographic) analysis method for detecting DEAB and MK in printing and packaging material
CN103675153A (en) * 2013-12-26 2014-03-26 国家烟草质量监督检验中心 Method for measuring main carbonyl compounds in cigarette filter through ultra-performance convergence chromatography
CN103698458A (en) * 2013-12-26 2014-04-02 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
CN103837635A (en) * 2014-03-27 2014-06-04 中国热带农业科学院农产品加工研究所 Method for determining content of biogenic amines in foods by adopting ultra-efficient bonded phase chromatography
CN104133023A (en) * 2014-08-25 2014-11-05 国家烟草质量监督检验中心 Analysis method for simultaneously detecting tralomethrin and deltamethrin in tobaccos by using bonded phase chromatography
CN104181246A (en) * 2014-08-25 2014-12-03 国家烟草质量监督检验中心 Convergence chromatography analytical method for residue of herbicides in tobacco
CN104914182A (en) * 2015-05-29 2015-09-16 安徽古井贡酒股份有限公司 Method for rapidly detecting four vitamins E in white spirit simultaneously by utilizing ultra performanceconvergence chromatography
CN105067733A (en) * 2015-07-16 2015-11-18 中国热带农业科学院农产品加工研究所 Method for measuring content of vitamin E in food with ultra-performance convergence chromatography

Patent Citations (8)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103499668A (en) * 2013-09-30 2014-01-08 国家烟草质量监督检验中心 UPC<2> (ultra performance convergence chromatographic) analysis method for detecting DEAB and MK in printing and packaging material
CN103675153A (en) * 2013-12-26 2014-03-26 国家烟草质量监督检验中心 Method for measuring main carbonyl compounds in cigarette filter through ultra-performance convergence chromatography
CN103698458A (en) * 2013-12-26 2014-04-02 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
CN103837635A (en) * 2014-03-27 2014-06-04 中国热带农业科学院农产品加工研究所 Method for determining content of biogenic amines in foods by adopting ultra-efficient bonded phase chromatography
CN104133023A (en) * 2014-08-25 2014-11-05 国家烟草质量监督检验中心 Analysis method for simultaneously detecting tralomethrin and deltamethrin in tobaccos by using bonded phase chromatography
CN104181246A (en) * 2014-08-25 2014-12-03 国家烟草质量监督检验中心 Convergence chromatography analytical method for residue of herbicides in tobacco
CN104914182A (en) * 2015-05-29 2015-09-16 安徽古井贡酒股份有限公司 Method for rapidly detecting four vitamins E in white spirit simultaneously by utilizing ultra performanceconvergence chromatography
CN105067733A (en) * 2015-07-16 2015-11-18 中国热带农业科学院农产品加工研究所 Method for measuring content of vitamin E in food with ultra-performance convergence chromatography

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
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

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