CN105954428A - Determination method for carbon, hydrogen and nitrogen stable isotope ratios of nicotine in boletus edulis - Google Patents

Determination method for carbon, hydrogen and nitrogen stable isotope ratios of nicotine in boletus edulis Download PDF

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CN105954428A
CN105954428A CN201610518597.8A CN201610518597A CN105954428A CN 105954428 A CN105954428 A CN 105954428A CN 201610518597 A CN201610518597 A CN 201610518597A CN 105954428 A CN105954428 A CN 105954428A
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nicotine
bolete
stable isotope
nitrogen
hydrogen
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韩书磊
陈欢
马潇
付亚宁
刘彤
侯宏卫
胡清源
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National Tobacco Quality Supervision and Inspection Center
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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
    • 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
    • G01N2030/022—Column chromatography characterised by the kind of separation mechanism
    • G01N2030/025—Gas chromatography

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Abstract

The invention provides a determination method for carbon, hydrogen and nitrogen stable isotope ratios of nicotine in boletus edulis. The determination method is characterized in that after the nicotine in the boletus edulis is extracted by adopting an n-hexane/sodium hydroxide water solution system, an extracting solution is purified through cation exchange solid-phase extraction; the nicotine is separated from other impurities in the extracting solution by adopting a gas chromatograph provided with a capillary chromatographic column; the carbon stable isotope ratio delta13C, the hydrogen stable isotope ratio deltaD and the nitrogen stable isotope ratio delta15N of the nicotine in the boletus edulis are analyzed by adopting a gas chromatograph-isotope ratio mass spectrometer (GC-IRMS); delta12C, deltaD and delta15N of the nicotine in the boletus edulis are calibrated and calculated according to determination values of delta12C, deltaD and delta15N in isotopic standard materials of the nicotine. By adopting a GC-IRMS technology, accurate determination of the carbon, hydrogen and nitrogen stable isotope ratios of the nicotine in the boletus edulis is realized and technical supports and scientific evidences are provided for tracing the source of the nicotine in related products.

Description

Nicotine carbon, hydrogen, the assay method of nitrogen Stable isotope ratio in bolete
Technical field
The invention belongs to Stable Isotopic Analysis technical field, be specifically related to nicotine carbon in a kind of bolete, hydrogen, nitrogen stable The assay method of isotopic ratio.
Background technology
Currently, it is determined that the source of nicotine in commercially available tobacco extract and different purity nicotine, have great importance.Smoke abatement Outside grass, the crop such as bolete also contains nicotine, although the nicotine content of bolete is the lowest, but with other Solanaceae class plant phases Ratio, its nicotine content is of a relatively high, so, bolete is one of important sources of nicotine in nature.Currently, many commercially available rings Smoke product, electronic cigarette, health promoting product etc. all contain nicotine, but, for the source of wherein nicotine, there is no unified final conclusion.So, The exploitation of nicotine tracing technology, has important theory and realistic meaning.
In the method traced to the source in product variety, the place of production etc., stable isotope technology is the analysis means of a relative efficiency. Due to the isotopics climate in organism, the impact of the factors such as environment and biological metabolism type, variety classes and difference In the raw-food material in source, region, isotope natural abundance there are differences, and utilizes this species diversity can be to variety classes and source Product carry out tracing to the source (woods radiance, stable isotope is ecological. Higher Education Publishing House, 2013).But, have not yet to see cattle Nicotine carbon, hydrogen, the relevant report of nitrogen Stable isotope ratio in liver bacterium.
Summary of the invention
The purpose of the present invention is based on above-mentioned technological gap, establishes nicotine carbon, hydrogen, nitrogen in a kind of bolete stably same The assay method of position element ratio.Nicotine in bolete extracted by this method by the process such as liquid-liquid extraction, Solid-Phase Extraction, Concentrate and purify, and a sample pretreatment process can measure the carbon of nicotine in bolete, hydrogen, nitrogen stable isotope ratio simultaneously Value.
It is an object of the invention to be achieved through the following technical solutions: in a kind of bolete nicotine carbon, hydrogen, nitrogen stably with The assay method of position element ratio, after using normal hexane/sodium hydrate aqueous solution system to be extracted by the nicotine in bolete, then Through cation exchange Solid-Phase Extraction, extract is purified, and employing is furnished with the gas chromatograph of capillary chromatographic column by cigarette Other impurity in alkali and extract separately, utilizes gas chromatogram isotope mass spectrometer GC-IRMS to analyze nicotine in bolete Carbon stable isotope ratio delta13C, hydrogen stable isotope ratio delta D and nitrogen Stable isotope ratio δ15N, further according to nicotine coordination δ in element standard substance12C, δ D and δ15N measured value, the δ of nicotine in calibration calculations bolete12C, δ D and δ15N value.
It specifically comprises the following steps that
(1) nicotine in bolete extraction, concentrate and purify: use normal hexane/sodium hydrate aqueous solution system by bolete In nicotine extract after, then through cation exchange Solid-Phase Extraction nicotine is purified；
(2) gas chromatograph with capillary gas chromatographic column is used to be separated with other impurity in extract by nicotine；
(3) with online burner, the C in nicotine is changed into CO2, the N in nicotine is changed into N2, use isotope mass spectrometer (IRMS) measure nicotine and produce CO2In δ13C and N2In δ15N value；
(4) online burner is switched to thermal transition pattern, measure nicotine with isotope mass spectrometer (IRMS) and produce H2In δ D value (i.e. δ2H).
(5) δ demarcated by standard substance13C, δ D and δ15N value, obtains the δ of nicotine in bolete13C, δ D and δ15N Value.
Extraction in step (1) is as follows with purification process:
Extract: weigh about 5 g bolete samples, be placed in 50 mL centrifuge tubes, be separately added into 30 mL 1% sodium hydrate aqueous solutions With 5 mL normal hexane, under 2000 rpm after vortex 10 min, under 10000 rpm, centrifugal 2 min, are transferred to upper organic phase In another 50 mL centrifuge tube, then with 5 mL n-hexane extraction twice, merge organic facies；
Concentrate, purify: with formic acid, the pH value of organic facies is adjusted to 3-4, then at 40 DEG C, its nitrogen is blown concentration and closely does, add 3 After mL 2% aqueous formic acid dissolved residue, use cation exchange solid phase extraction column (60 mg, Waters Oasis MCX) Carry out purified treatment, the steps include: that extraction column is lived with 3 mL methanol, 3 mL water and 3 mL 2% aqueous formic acids before using respectively Change, afterwards solution to be clean is transferred in post, successively with 3 mL water and 3 mL methanol drip washing, then by 10 mL 5% ammonification first Alcohol eluting, collects eluent；Eluent formic acid adjusts pH value to 3-4, and at 40 DEG C, nitrogen blows and concentrates near doing, residue 5% sodium hydroxide Aqueous solution adjusts pH value to alkalescence, adds 1.5 mL dichloromethane, under 2000 rpm after vortex 2 min, is centrifuged with 10000 rpm 1 min, then take organic facies and carry out GC-IRMS analysis.
The instrumental conditions of described method is:
(1) GC conditions:
Chromatographic column: middle polarity capillary chromatographic column (30 mm × 0.25, m × 0.32 μm)；Detector temperature: 250 ℃；Injector temperature: 250 DEG C；Carrier gas: nitrogen (purity >=99.999%), constant current flow velocity: 2.0 mL/min；Sample size: 1 μ L, Splitless injecting samples；Heating schedule: initial temperature 80 DEG C, keeps 1 min, with the speed of 15 DEG C/min to 260 DEG C, keeps 6 min.
(2) burning conversion device condition:
Measure δ13C or δ15N: using oxidizing fire pipe, arranging temperature is 1000 DEG C.Nickel/nickel oxide (Ni/NiO) is loaded in pipe, Weak oxidant made by nickel oxide, and the C in sample is oxidized to CO2, N in sample is oxidized to NxOy, meanwhile, nickel oxide is converted into nickel Simple substance, is filled with O2Renewable nickel oxide, it addition, nickel simple substance can make special reducing agent, by NxOyIt is converted into N2, sample end reaction Generate CO2And N2.Oxidizing fire pipe should inject O before using2 Regeneration for oxidation tube in one hour.
Measure δ15N, need to use liquid nitrogen cold trap to freeze to remove CO2High-solidification point gas, prevents CO2Enter ion source and get broken Sheet ion [CO+] m/z 28,29 is to [N2+] m/z 28,29 interferes.
Measure δ D: using Pintsch process pipe, arranging temperature is 1450 DEG C.Pintsch process pipe should inject CH before using4One Hour for reaction tube utter misery.
(3) Mass Spectrometry Conditions is:
Ion source vacuum is 1.8x 10-6 MBar, voltage 3.04 kV, electric current 1.50 mA.
Nicotine in bolete is extracted, concentrates by steps such as liquid-liquid extraction, cation exchange Solid-Phase Extraction by this method And purification, and a sample pretreatment process can measure the carbon of nicotine in bolete, hydrogen, nitrogen Stable isotope ratio simultaneously, There is the advantage that efficiency is high, reproducible, provide technical support and scientific basis for tracing to the source of nicotine in tobacco extract.
Accompanying drawing explanation
Fig. 1 is δ in GC-IRMS bioassay standard solution nicotine13The ion flow graph spectrum of C, upper figure vertical coordinate is ratio (Ratio), figure below vertical coordinate is intensity (Intensity [mV]);
Fig. 2 is δ in GC-IRMS bioassay standard solution nicotine15The ion flow graph spectrum of N, upper figure vertical coordinate is ratio (Ratio), figure below vertical coordinate is intensity (Intensity [mV]);
Fig. 3 is the ion flow graph spectrum of δ D in GC-IRMS bioassay standard solution nicotine, and upper figure vertical coordinate is ratio (Ratio), Figure below vertical coordinate is intensity (Intensity [mV]).
Detailed description of the invention
The present invention is further described by specific examples below, but is not intended to the present invention.
Embodiment 1:
1, instrument and reagent
Isotope mass spectrometer (AS1310 automatic sampler, Trace GC Ultra gas chromatograph, GC IsoLink burning and heat Reforming unit (burner is used for measuring the carbon in nicotine and nitrogen, and heat conversion device is used for measuring the hydrogen in nicotine), Delta V Advantage stable isotope compares mass spectrograph.Thermo Fisher company of the U.S.)；AE163 electronic balance (sensibility reciprocal: 0.0001 G, Mettler company of Switzerland)；Full-automatic Nitrogen evaporator (model: JTZD-DCY12S, same Electronics Co., Ltd. is gathered in Hangzhou)；High speed powder Broken machine (Wuhan Yin Cai Science and Technology Ltd.)；Vortex oscillator (U.S. Coleparmer Votex-Genie)；High speed desktop is cold Freeze type centrifuge (Germany SIGMA 3-30K)；High-purity helium (99.999%, carrier gas)；Nicotine standard substance comes from U.S.'s print the An Na university isotopic laboratory, #2(δ13C=7.72 ± 0.02 ‰, δ15N=-5.94 ± 0.15 ‰), #3(δ13C =-30.05 ± 0.02 ‰, δ15N=-33.62 ± 0.18 ‰), #4(δ13C=-2.06 ± 0.02 ‰, δ15N=-15.49 ± 0.13 ‰), #5(δ13C=-29.63 ± 0.01 ‰, δ15N=--6.03 ± 0.04 ‰, δ D=-161.30 ± 1.7 ‰)；Normal hexane (chromatographically pure, the U.S. TEDIA company)；Sodium hydroxide (analytical pure, traditional Chinese medicines group)；Ultra-pure water (Milli-Q Integral ultrapure water system system)；Sun Ion Exchange Solid Phase extraction pillar (60 mg, Waters Oasis MCX).
2, sample pre-treatments
(1) bolete sample is placed in 40oIn C baking oven, take out after 1 hour, after pulverizing, cross 0.45 mm pore size standard screen；
(2) weigh about 5 g bolete samples, be placed in 50 mL centrifuge tubes, be separately added into 30 mL 1% sodium hydrate aqueous solutions and 5 mL normal hexane, under 2000 rpm after vortex 10 min, under 10000 rpm, centrifugal 2 min, are transferred to upper organic phase separately In one 50 mL centrifuge tube, then with 5 mL n-hexane extraction twice, merge organic facies.
(3) with formic acid, the pH value of organic facies is adjusted to 3-4, then at 40 DEG C, its nitrogen is blown concentration and closely does, add 3 mL After 2% aqueous formic acid dissolved residue, cation exchange solid phase extraction column (60 mg, Waters Oasis MCX) is used to carry out Purified treatment, the steps include: that extraction column activates with 3 mL methanol, 3 mL water and 3 mL 2% aqueous formic acids before using respectively, it After solution to be clean is transferred in post, successively with 3 mL water and 3 mL methanol drip washing, then wash with 10 mL 5% ammoniated methanol De-, collect eluent；Eluent formic acid adjusts pH value to 3-4, and at 40 DEG C, nitrogen blows and concentrates near doing, and residue is water-soluble with 5% sodium hydroxide Liquid adjusts pH value to alkalescence, adds 1.5 mL dichloromethane, under 2000 rpm after vortex 2 min, is centrifuged 1 with 10000 rpm Min, then take organic facies and carry out GC-IRMS analysis.
% in this case unless otherwise noted, is quality %.
3, instrumental conditions
(1) GC conditions:
Chromatographic column: middle polarity capillary chromatographic column (30 mm × 0.25, m × 0.32 μm)；Detector temperature: 250 ℃；Injector temperature: 250 DEG C；Carrier gas: nitrogen (purity >=99.999%), constant current flow velocity: 2.0 mL/min；Sample size: 1 μ L, split ratio: 10:1；Heating schedule: initial temperature 80 DEG C, keeps 1 min, with the speed of 15 DEG C/min to 260 DEG C, keeps 6 min.
(2) burning conversion device condition:
Measure δ13C or δ15N: using oxidizing fire pipe, arranging temperature is 1000 DEG C.Nickel/nickel oxide (Ni/NiO) is loaded in pipe, Weak oxidant made by nickel oxide, and the C in sample is oxidized to CO2, N in sample is oxidized to NxOy, meanwhile, nickel oxide is converted into nickel Simple substance, is filled with O2Renewable nickel oxide, it addition, nickel simple substance can make special reducing agent, by NxOyIt is converted into N2, sample end reaction Generate CO2And N2.Oxidizing fire pipe should inject O before using2 Regeneration for oxidation tube in one hour.
Measure δ15N, need to use liquid nitrogen cold trap to freeze to remove CO2High-solidification point gas, prevents CO2Enter ion source and get broken Sheet ion [CO+] m/z 28,29 is to [N2+] m/z 28,29 interferes.
Measure δ D: using Pintsch process pipe, arranging temperature is 1450 DEG C.Pintsch process pipe should inject CH before using4One Hour for reaction tube utter misery.
(3) Mass Spectrometry Conditions is:
Ion source vacuum is 1.8x 10-6 MBar, voltage 3.04 kV, electric current 1.50 mA.
4, precision measures
After bolete diluted sample is extracted, by the δ of nicotine in GC-IRMS technology replication bolete of the present invention13C, δ D and δ15N value (n=6), the relative standard deviation (RSD) of measurement result respectively 1.16%, 0.36% and 1.02%(table 1), measurement accuracy all can reach requirement.
In table 1. bolete, the precision of tri-kinds of elemental stable isotopes ratios of nicotine C, H, N measures
According to above-mentioned GC-IRMS assay method, record the δ of nicotine in bolete sample13C, δ D and δ15N respectively-30.82 ,- 215.60 and-9.54.

Claims (5)

1. nicotine carbon, hydrogen, the assay method of nitrogen Stable isotope ratio in a bolete, it is characterised in that: employing normal hexane/ After nicotine in bolete is extracted by sodium hydrate aqueous solution system, then through cation exchange Solid-Phase Extraction to extract Purify, and use the gas chromatograph being furnished with capillary chromatographic column to be separated with other impurity in extract by nicotine, profit The carbon stable isotope ratio delta of nicotine in bolete is analyzed with gas chromatogram isotope mass spectrometer GC-IRMS13C, stabilized hydrogen is same Position element ratio delta D and nitrogen Stable isotope ratio δ15N, further according to the δ in nicotine isotopic standard material12C, δ D and δ15N measures Value, the δ of nicotine in calibration calculations bolete12C, δ D and δ15N value.
Nicotine carbon, hydrogen, the assay method of nitrogen Stable isotope ratio, its feature in bolete the most according to claim 1 It is: specifically comprising the following steps that of the method
(1) nicotine in bolete extraction, concentrate and purify: use normal hexane/sodium hydrate aqueous solution system by bolete In nicotine extract after, then through cation exchange Solid-Phase Extraction nicotine is purified；
(2) gas chromatograph with capillary gas chromatographic column is used to be separated with other impurity in extract by nicotine；
(3) with online burner, the C in nicotine is changed into CO2, the N in nicotine is changed into N2, use isotope mass spectrometer (IRMS) measure nicotine and produce CO2In δ13C and N2In δ15N value；
(4) online burner is switched to thermal transition pattern, measure nicotine with isotope mass spectrometer IRMS and produce H2In δ D Value；
(5) δ demarcated by standard substance13C, δ D and δ15N value, obtains the δ of nicotine in bolete13C, δ D and δ15N value.
Nicotine carbon, hydrogen, the assay method of nitrogen Stable isotope ratio, its feature in bolete the most according to claim 1 It is: the extraction in step (1) is as follows with purification process:
Extract: weigh 5 g bolete samples, be placed in 50 mL centrifuge tubes, be separately added into 30 mL 1% sodium hydrate aqueous solutions and 5 mL normal hexane, under 2000 rpm after vortex 10 min, under 10000 rpm, centrifugal 2 min, are transferred to upper organic phase separately In one 50 mL centrifuge tube, then with 5 mL n-hexane extraction twice, merge organic facies；
Concentrate, purify: with formic acid, the pH value of organic facies is adjusted to 3-4, then at 40 DEG C, its nitrogen is blown concentration and closely does, add 3 After mL 2% aqueous formic acid dissolved residue, use cation exchange solid phase extraction column to carry out purified treatment, the steps include: extraction Take and activate with 3 mL methanol, 3 mL water and 3 mL 2% aqueous formic acids respectively before post uses, afterwards solution to be clean is transferred to In post, successively with 3 mL water and 3 mL methanol drip washing, then with 10 mL 5% ammoniated methanol eluting, collect eluent；Eluent Adjusting pH value to 3-4 with formic acid, at 40 DEG C, nitrogen blows and concentrates near doing, and residue adjusts pH value to alkaline with 5% sodium hydrate aqueous solution, adds 1.5 mL dichloromethane, under 2000 rpm after vortex 2 min, are centrifuged 1 min with 10000 rpm, then take organic facies and carry out GC- IRMS analyzes.
Nicotine carbon, hydrogen, the assay method of nitrogen Stable isotope ratio, its feature in bolete the most according to claim 2 It is: the GC conditions in step (2) is:
Chromatographic column: middle polarity capillary chromatographic column, mm × 0.25, specification 30 m × 0.32 μm；Detector temperature: 250 ℃；Injector temperature: 250 DEG C；Carrier gas: nitrogen, constant current flow velocity: 2.0 mL/min；Sample size: 1 μ L, split ratio: 10:1, surveys Determine δ D and δ15Not shunt mode is used during N；Heating schedule: initial temperature 80 DEG C, keeps 1 min, with the speed of 15 DEG C/min To 260 DEG C, keep 6 min.
Nicotine carbon, hydrogen, the assay method of nitrogen Stable isotope ratio, its feature in bolete the most according to claim 2 It is: the online burner condition used by step (3), (4) is:
Measure δ13C or δ15N: using oxidizing fire pipe, arranging temperature is 1000 DEG C, loads nickel/nickel oxide (Ni/NiO) in pipe, Weak oxidant made by nickel oxide, and the C in sample is oxidized to CO2, N in sample is oxidized to NxOy, meanwhile, nickel oxide is converted into nickel Simple substance, is filled with O2Renewable nickel oxide, it addition, nickel simple substance can make special reducing agent, by NxOyIt is converted into N2, sample end reaction Generate CO2And N2, oxidizing fire pipe should inject O before using2 Regeneration for oxidation tube in one hour；
Measure δ15N, need to use liquid nitrogen cold trap to freeze to remove CO2High-solidification point gas, prevents CO2Enter ion source get fragment from Son [CO+] m/z 28,29 is to [N2+] m/z 28,29 interferes；
Measuring δ D: using Pintsch process pipe, arranging temperature is 1450 DEG C, Pintsch process pipe should inject CH before using4One hour with In reaction tube utter misery.
CN201610518597.8A 2016-07-05 2016-07-05 Determination method for carbon, hydrogen and nitrogen stable isotope ratios of nicotine in boletus edulis Pending CN105954428A (en)

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CN107064385A (en) * 2017-04-13 2017-08-18 国家烟草质量监督检验中心 The extraction of N nitrosamine and assay method in a kind of bolete that SPE is exchanged based on hydrophobic nonionic
CN111983048A (en) * 2020-07-10 2020-11-24 广东工业大学 Method for determining nitrogen stable isotope of organic amine monomer and application thereof
CN113933372A (en) * 2021-11-11 2022-01-14 广西大学 Method for quantitatively identifying river entering load and river entering coefficient of river basin nitrate nitrogen source

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CN107064385A (en) * 2017-04-13 2017-08-18 国家烟草质量监督检验中心 The extraction of N nitrosamine and assay method in a kind of bolete that SPE is exchanged based on hydrophobic nonionic
CN111983048A (en) * 2020-07-10 2020-11-24 广东工业大学 Method for determining nitrogen stable isotope of organic amine monomer and application thereof
CN113933372A (en) * 2021-11-11 2022-01-14 广西大学 Method for quantitatively identifying river entering load and river entering coefficient of river basin nitrate nitrogen source
CN113933372B (en) * 2021-11-11 2023-11-03 广西大学 Quantitative identification method for river basin nitrate nitrogen source river entering load and river entering coefficient

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