CN106290682B - Chiral analysis method of nicotine in tea - Google Patents

Chiral analysis method of nicotine in tea Download PDF

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CN106290682B
CN106290682B CN201610667779.1A CN201610667779A CN106290682B CN 106290682 B CN106290682 B CN 106290682B CN 201610667779 A CN201610667779 A CN 201610667779A CN 106290682 B CN106290682 B CN 106290682B
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nicotine
tea
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CN106290682A (en
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李小兰
周芸
刘鸿
黄善松
林莉
许蔼飞
蒋宏霖
蒋光辉
周奕
潘玉灵
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China Tobacco Guangxi Industrial Co Ltd
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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
    • G01N30/88Integrated 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
    • G01N30/04Preparation 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
    • G01N30/64Electrical detectors
    • G01N30/68Flame ionisation detectors
    • 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
    • G01N30/78Detectors specially adapted therefor using more than one detector
    • 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
    • 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
    • G01N30/64Electrical detectors
    • G01N2030/685Electrical detectors flame photometry
    • 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
    • G01N2030/884Integrated analysis systems specially adapted therefor, not covered by a single one of the groups G01N30/04 - G01N30/86 analysis specially adapted for the sample organic compounds

Abstract

The invention discloses a chiral analysis method of nicotine in tea, which is characterized by comprising the following steps: drying, crushing and sieving a tea sample, adding an extraction liquid for extraction and filtering, performing multi-dimensional gas chromatography-tandem mass spectrometry after automatic solid-phase microextraction, and quantitatively detecting the proportion of S- (-) -nicotine and R- (+) -nicotine in the tea by adopting a peak area normalization method. The detection method provided by the method has the advantages of simple and rapid sample treatment, low detection limit, high sensitivity and good precision, and can meet the requirement of chiral analysis of nicotine in the tea sample.

Description

Chiral analysis method of nicotine in tea
Technical Field
The invention relates to a method for measuring chemical components of tea, in particular to a chiral analysis method of nicotine in tea.
Background
Nicotine, also called nicotine, is an alkaloid present in solanaceae plants and is also an important component of tobacco, and studies have shown that the tea leaves also contain nicotine at a level of about 163-1600 mug/kg. The nicotine molecule contains one chiral center, the 2-carbon atom on the tetrahydropyrrole ring, so that nicotine has two enantiomers: s- (-) -nicotine and R- (+) -nicotine. The two enantiomers of nicotine have completely different contents, metabolic mechanisms and physiological properties. The physiological activity and toxicity of S- (-) -nicotine are higher than those of R- (+) -nicotine, for example, S- (-) -nicotine has 10 to 100 times higher affinity than R- (+) -nicotine with respect to nicotinic acetylcholine receptor. Therefore, performing chiral analysis of nicotine in tea leaves is of great importance to understand the health risks of nicotine intake through tea leaves.
At present, chiral analysis of nicotine mainly aims at research on chiral analysis methods of nicotine in tobacco and tobacco products, and no chiral analysis method of nicotine in tea leaves is available. The content of nicotine in tea leaves is far lower than that in tobacco, which brings a challenge to chiral analysis of nicotine in tea leaves. Therefore, it is necessary to develop a method for accurately quantifying S- (-) -nicotine and R- (+) -nicotine in tea leaves with high sensitivity and high precision.
Disclosure of Invention
The invention provides a chiral analysis method of nicotine in tea.
The method takes nicotine as a research object, carries out pretreatment method research on tea samples, establishes an analysis method of nicotine optical isomers in the tea based on an automatic solid-phase microextraction-multidimensional gas chromatography-mass spectrometry system, and realizes accurate determination of nicotine optical enantiomers S- (-) -nicotine and R- (+) -nicotine in the tea.
The purpose of the invention is realized by the following technical scheme: a chiral analysis method of nicotine in tea comprises drying tea sample, pulverizing, sieving, adding extractive solution, extracting, filtering, performing automatic solid phase microextraction, and performing multidimensional gas chromatography tandem mass spectrometry (MDGCMS) analysis.
The scheme of the application comprises the following steps: 1) preparing a standard solution; 2) uniformly mixing tea samples; 3) extracting a tea sample; 4) multidimensional gas chromatography-tandem mass spectrometry; 5) and performing qualitative analysis on S- (-) -nicotine and R- (+) -nicotine by using retention time of nicotine chromatographic peaks of a reference standard sample and a tea leaf sample and characteristic ions, and performing normalized quantification on the peak area of the quantitative ions to obtain the proportion of the S- (-) -nicotine and the R- (+) -nicotine in the total nicotine.
The preferred scheme of the invention comprises the following specific steps:
1) preparation of a standard solution: 100.0mg of S- (-) -nicotine standard and 50.0mg of R- (+) -nicotine standard were weighed, and mixed standard solutions of S- (-) -nicotine and R- (+) -nicotine at concentrations of 100. mu.g/mL and 50. mu.g/mL, respectively, S- (-) -nicotine standard solution at a concentration of 100. mu.g/mL, and R- (+) -nicotine standard solution at a concentration of 100. mu.g/mL were prepared using n-hexane.
2) And (3) uniformly mixing tea samples: placing the tea sample in a drying oven at 40 ℃, taking out the tea sample after 1 hour, and sieving the tea sample through a standard sieve with the aperture of 0.45 mm after crushing;
3) extraction of tea samples: weighing about 5g of tea powder, placing the tea powder in a 100mL conical flask, adding 20mL of water, 40mL of n-hexane and 10mL of 2mol/L sodium hydroxide solution, shaking and extracting for 1 hour with a plug, and standing the extract for 30min in a dark place; taking the upper organic phase, centrifuging at 2000g for 10min, and filtering with 0.22 μm filter membrane to give sample.
4) Multidimensional gas chromatography tandem mass spectrometry: carrying out automatic solid-phase microextraction on the filtrate obtained in the step 3), and then carrying out multidimensional gas chromatography-tandem mass spectrometry on the filtrate under the following specific conditions:
① automatic solid phase microextraction conditions:
the automatic extraction fiber needs to be aged when being used for the first time, and the conditions are as follows:
stationary phase PDMS/DVB (polydimethylsiloxane/divinylbenzene), aging at 250 deg.C for 30 min;
heating the sample at 30 deg.C, preheating for 3min, extracting for 5min, desorbing for 5min, injecting sample, and baking needle at 250 deg.C for 10 min.
② one-dimensional analysis conditions:
a chromatographic column: 30 m.times.0.25 mm.times.0.25 μm 5% diphenyl-95% dimethylpolysiloxane capillary chromatography column.
Sample inlet temperature: at 250 ℃ to obtain a mixture.
Carrier gas: helium (purity is more than or equal to 99.999%), constant pressure sample injection: 117.9 kPa.
Temperature rising procedure: the initial temperature is 80 deg.C, the equilibration time is 1min, the temperature is increased to 200 deg.C at a rate of 10 deg.C/min, and the temperature is maintained for 10 min.
A detector: flame Ionization Detector (FID); temperature: 280 ℃; hydrogen gas: 40 mL/min; air: 400 mL/min; tail blowing: 10 mL/min; the cutting pressure was 50.0 kPa.
③ two-dimensional analysis conditions:
a chromatographic column: 30 m.times.0.25 mm.times.0.25 μm cyclodextrin capillary chromatography column.
Temperature rising procedure: the initial temperature was 50 ℃ and held for 3min, ramping up to 130 ℃ at a rate of 2 ℃/min, then ramping up to 180 ℃ at a rate of 3 ℃/min and held for 1 min.
A detector: an electron impact source (EI); ion source temperature: 200 ℃; interface temperature: 220 ℃; the detector voltage is 0kV with respect to the tuning result; solvent retardation: 3 min; detection mode: selecting an ion detection mode (SIM); ions 84 are quantified.
5) And performing qualitative analysis on S- (-) -nicotine and R- (+) -nicotine by using retention time of nicotine chromatographic peaks of a reference standard sample and a tea leaf sample and characteristic ions, and performing normalized quantification on the peak area of the quantitative ions to obtain the proportion of the S- (-) -nicotine and the R- (+) -nicotine in the total nicotine.
Step 1) the preparation of the standard solution is more preferably: weighing about 100.0mg of S- (-) -nicotine standard, diluting with n-hexane, diluting to a constant volume into a 50mL brown volumetric flask, and preparing S- (-) -nicotine standard stock solution with a concentration of about 2.0 mg/mL; weighing about 50.0mg of R- (+) -nicotine standard substance, diluting with n-hexane, diluting to constant volume to 50mL of brown volumetric flask, and preparing into R- (+) -nicotine standard stock solution with concentration of about 1.0 mg/mL; diluting with S- (-) -nicotine standard stock solution and R- (+) -nicotine standard stock solution to prepare mixed standard solutions with S- (-) -nicotine and R- (+) -nicotine concentrations of 100 μ g/mL and 50 μ g/mL respectively, and diluting to obtain S- (-) -nicotine and R- (+) -nicotine standard solutions of 100 μ g/mL respectively.
The capillary column in the one-dimensional analysis in step 4) is an Rtx-5MS chromatographic column or is replaced by a corresponding equivalent column.
The cyclodextrin capillary chromatographic column in the two-dimensional analysis in step 4) is an InertCap CHIRAMIX chromatographic column or is replaced by a corresponding equivalent column.
The invention provides a chiral analysis method of nicotine in tea, which has the following excellent effects:
1. the method adopts the pretreatment methods of liquid-liquid extraction and solid-phase microextraction, and has the advantages of simple pretreatment process, simple and rapid operation and good pretreatment effect.
2. The method adopts a multidimensional gas phase gas chromatography-mass spectrometry system, can realize better separation of S- (-) -nicotine and R- (+) -nicotine, has a detection Limit (LOD) of the R- (+) -nicotine of 0.25 percent, and can meet the chiral analysis of the nicotine in the tea sample.
3. The method adopts the mass spectrum with high sensitivity and strong anti-interference capability for detection, so the method has the advantages of accurate operation, low detection limit, good recovery rate and repeatability and the like.
Drawings
FIG. 1 is a chromatogram of a mixed standard solution
FIG. 2 is a chromatogram of tea leaf sample No. 1
Detailed Description
The invention is further described by the following specific examples, but is not limited thereto.
1. Instruments and reagents
MDGCMS-QP2010Ultra multidimensional gas chromatograph-mass spectrometer (Shimadzu, Japan), autosampler AOC-5000 (Shimadzu, Japan), autosolidification micro-extraction fiber needle, 65 μm PDMS/DVB (polydimethylsiloxane/divinylbenzene) stationary phase extraction fiber head (Supelco, USA), Rtx-5MS column (30m × 0.25mm × 0.25 μm, Shimadzu, Japan), InertCap CHIRAMIX column (30m × 0.25mm × 0.25 μm, Shimadzu, Japan), AE163 electronic balance (sensitivity: 0.0001g, Mettler, Switzerland, HY-8 adjustable oscillator (Kimura electric appliances, Inc., U.A.), high speed pulverizer (silver science Co., Ltd., Wuhan), SIGMA 3-30K-high speed desk type refrigerated centrifuge, Germany. N-hexane (chromatographic purity), sodium hydroxide (analytical purity), S- (-) -nicotine standard (CAS: 54-11-5), R- (+) -nicotine standard (CAS: 25162-00-9).
2. Preparation of Standard solutions
Weighing about 100.0mg of S- (-) -nicotine standard, diluting with n-hexane, diluting to a constant volume into a 50mL brown volumetric flask, and preparing S- (-) -nicotine standard stock solution with a concentration of about 2.0 mg/mL; weighing about 50.0mg of R- (+) -nicotine standard substance, diluting with n-hexane, diluting to constant volume to 50mL of brown volumetric flask, and preparing into R- (+) -nicotine standard stock solution with concentration of about 1.0 mg/mL; respectively taking 50 mu L S- (-) -nicotine standard stock solution and R- (+) -nicotine standard stock solution, diluting with n-hexane to constant volume to 100mL brown volumetric flasks, preparing mixed standard solutions with S- (-) -nicotine and R- (+) -nicotine concentrations of 1 mu g/mL and 0.5 mu g/mL respectively, and additionally respectively diluting the standard stock solutions to obtain S- (-) -nicotine and R- (+) -nicotine standard solutions with 1 mu g/mL.
3. Chiral analysis of nicotine standard solutions
And taking 10mL of mixed standard solution for sample injection analysis according to the automatic solid-phase microextraction-multidimensional gas-phase gas-mass analysis condition. The results show that better separation of S- (-) -nicotine and R- (+) -nicotine can be achieved under the conditions; taking 10mL of S- (-) -nicotine standard solution to perform automatic solid phase microextraction-multidimensional gas phase gas quality analysis, further performing multidimensional gas phase gas quality analysis on 10mL of R- (+) -nicotine standard solution, and finally determining that S- (-) -nicotine is prior to R- (+) -nicotine to generate peaks through the retention time of S- (-) -nicotine and R- (+) -nicotine.
Detection limits for R- (+) -Nicotine
The chiral composition of nicotine is generally expressed as a percentage of R- (+) -nicotine to total nicotine. To assess the detection limit of R- (+) -nicotine, the method of the present invention adds a standard solution of R- (+) -nicotine to a standard solution of S- (-) -nicotine. The result shows that a response signal of R- (+) -nicotine can be observed in the S- (-) -nicotine standard solution, and after the peak area of the quantitative ion is normalized, the proportion of R- (+) -nicotine in the S- (-) -nicotine standard solution is 0.25% (the peak area is relative to the total nicotine peak area), so that the R- (+) -nicotine detection limit is used as the detection limit of the R- (+) -nicotine in the method.
5. Example of chiral analysis of Nicotine in tea samples
Placing the tea sample in a drying oven at 40 ℃, taking out the tea sample after 1 hour, and sieving the tea sample through a standard sieve with the aperture of 0.45 mm after crushing; weighing about 5g of tea powder, placing the tea powder in a 100mL conical flask, adding 20mL of water, 40mL of n-hexane and 10mL of 2mol/L sodium hydroxide solution, shaking and extracting for 1 hour with a plug, and standing the extract for 30min in a dark place; taking the upper organic phase, centrifuging at 2000g for 10min, filtering with 0.22 μm filter membrane, performing automatic solid phase microextraction, and performing multidimensional gas chromatography-tandem mass spectrometry; and performing qualitative analysis on S- (-) -nicotine and R- (+) -nicotine by using retention time of nicotine chromatographic peaks of a reference standard sample and a tea leaf sample and characteristic ions, and performing normalized quantification on the peak area of the quantitative ions to obtain the proportion of the S- (-) -nicotine and the R- (+) -nicotine in the total nicotine.
6 tea samples were analysed using this method and the results are shown in Table 1.
TABLE 1 chiral analysis of nicotine in tea
6. Precision of analytical methods
The same tea sample was taken for 5 day-within and day-between parallel determinations, and the precision of the method of the present invention was examined, with the results shown in tables 2 and 3. The result shows that the variation coefficients of the intra-day and the inter-day measurement results of the R- (+) -nicotine in the tea sample are 4.78% and 5.29%, respectively, and the precision is good.
TABLE 2 day precision of the test methods
TABLE 3 daytime precision of the test methods
The 6 tea samples were tested using the method of the specific embodiment. The chromatograms obtained by detection are shown in fig. 1 and fig. 2, wherein fig. 1 is the chromatogram of the mixed standard solution, and fig. 2 is the chromatogram of the tea leaf sample 1 #.

Claims (1)

1. A chiral analysis method of nicotine in tea is characterized in that: drying, crushing and sieving a tea sample, adding an extraction liquid for extraction and filtering, performing multi-dimensional gas chromatography-tandem mass spectrometry after automatic solid-phase microextraction, and quantitatively detecting the proportion of S- (-) -nicotine and R- (+) -nicotine in the tea by adopting a peak area normalization method; the method comprises the following specific steps:
1) preparation of a standard solution: weighing about 100.0mg of S- (-) -nicotine standard, diluting with n-hexane, diluting to a constant volume into a 50mL brown volumetric flask, and preparing S- (-) -nicotine standard stock solution with a concentration of about 2.0 mg/mL; weighing about 50.0mg of R- (+) -nicotine standard substance, diluting with n-hexane, diluting to constant volume to 50mL of brown volumetric flask, and preparing into R- (+) -nicotine standard stock solution with concentration of about 1.0 mg/mL; diluting the S- (-) -nicotine standard stock solution and the R- (+) -nicotine standard stock solution to prepare mixed standard solutions with the concentrations of the S- (-) -nicotine and the R- (+) -nicotine being 100 mug/mL and 50 mug/mL respectively, and diluting the mixed standard solutions respectively to obtain S- (-) -nicotine and R- (+) -nicotine standard solutions with the concentrations of 100 mug/mL;
2) and (3) uniformly mixing tea samples: placing the tea sample in a drying oven at 40 ℃, taking out the tea after 1 hour, and sieving the tea sample through a standard sieve with the aperture of 0.45 mm after crushing;
3) extraction of tea samples: weighing about 5g of tea powder, placing the tea powder in a 100mL conical flask, adding 20mL of water, 40mL of n-hexane and 10mL of 2mol/L sodium hydroxide solution, shaking and extracting for 1 hour with a plug, and standing the extract for 30min in a dark place; taking the upper organic phase, centrifuging at 2000g for 10min, and filtering with 0.22 μm filter membrane to give sample;
4) multidimensional gas chromatography tandem mass spectrometry: carrying out automatic solid-phase microextraction on the filtrate obtained in the step 3), and then carrying out multidimensional gas chromatography-tandem mass spectrometry on the filtrate under the following specific conditions:
① automatic solid phase microextraction conditions:
stationary phase: polydimethylsiloxane/divinylbenzene i.e. PDMS/DVB;
heating the sample at 30 deg.C, preheating for 3min, extracting for 5min, desorbing for 5min, and baking needle at 250 deg.C for 10min after sample injection;
② one-dimensional analysis conditions:
a chromatographic column: a 30m x 0.25mm x 0.25 μm Rtx-5MS chromatography column;
sample inlet temperature: 250 ℃;
carrier gas: helium with purity more than or equal to 99.999 percent, constant pressure sample injection: 117.9 kPa;
temperature rising procedure: the initial temperature is 80 ℃, the equilibrium time is 1min, the temperature is increased to 200 ℃ at the speed of 10 ℃/min, and the temperature is kept for 10 min;
a detector: flame Ionization Detector (FID); temperature: 280 ℃; hydrogen gas: 40 mL/min; air: 400 mL/min; tail blowing: 10 mL/min; the cutting pressure is 50.0 kPa;
③ two-dimensional analysis conditions:
a chromatographic column: an InertCap CHIRAMIX column of 30m × 0.25mm × 0.25 μm;
temperature rising procedure: the initial temperature is 50 ℃, the temperature is kept for 3min, the temperature is increased to 130 ℃ at the speed of 2 ℃/min, then the temperature is increased to 180 ℃ at the speed of 3 ℃/min, and the temperature is kept for 1 min;
a detector: an electron impact source (EI); ion source temperature: 200 ℃; interface temperature: 220 ℃; the detector voltage is 0kV with respect to the tuning result; solvent retardation: 3 min; detection mode: selecting an ion detection mode (SIM); quantifying the ion 84;
5) and performing qualitative analysis on S- (-) -nicotine and R- (+) -nicotine by using retention time of nicotine chromatographic peaks of a reference standard sample and a tea leaf sample and characteristic ions, and performing normalized quantification on the peak area of the quantitative ions to obtain the proportion of the S- (-) -nicotine and the R- (+) -nicotine in the total nicotine.
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CN107064381B (en) * 2017-03-10 2019-04-26 国家烟草质量监督检验中心 The chiral analysis of nicotine closes phase chromatographic tandem mass spectrography in a kind of tobacco and tobacco product
CN106841453A (en) * 2017-03-10 2017-06-13 国家烟草质量监督检验中心 The chiral analysis high performance liquid chromatography of nicotine in a kind of cigarette mainstream flue gas
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