CN108535389A - One grows tobacco the separation of middle NNN optical isomers and the conjunction phase chromatographic tandem mass spectrometry method that measures - Google Patents
One grows tobacco the separation of middle NNN optical isomers and the conjunction phase chromatographic tandem mass spectrometry method that measures Download PDFInfo
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Abstract
In growing tobacco the present invention relates to oneNNitrosonornicotine（NNN）The conjunction phase chromatographic tandem mass spectrometry method that optical isomer is detached and measured, belongs to tobacco chemistry analysis field.The present invention use containing 0.5% acetic acid methanol solution in tobacco sample (S) NNN and (R) NNN extracts, after extracting solution filtering, use UPC2MS/MS in extracting solution (S) NNN and (R) concentration of NNN analyzed and quantified.The sample pretreatment process of this method is simple, quick, is convenient for the analysis of batch sample.And when being detected with closing phase chromatographic tandem mass spectrum, used main mobile phase is supercritical fluid CO2, cosolvent use minimal amount of methanol, have the advantages that environmental-friendly.This detection method to (S) detection of NNN is limited to 0.21ng/mL, it is quantitatively limited to 0.69ng/mL, to (R) detection of NNN is limited to 0.34ng/mL, quantitatively it is limited to 1.12ng/mL.This method high sensitivity, it is reproducible, suitable for tobacco sampleNThe separation of nitrosonornicotine optical isomer and measurement.
Description
Technical field
In growing tobacco the present invention relates to oneNNitrosonornicotine（NNN）The conjunction phase chromatography that optical isomer is detached and measured
Tandem mass spectrum method belongs to tobacco chemistry analysis field.
Background technology
NNitrosonornicotine（NNN）It is the nitrosation of nicotiana alkaloids nornicotine in tobacco modulation and process
Effect and generate, have strong carcinogenicity, it is considered to be the major incentive of the cancer of the esophagus and carcinoma of mouth in smoking population.In its point
In minor structure, 2 carbon atoms on nafoxidine ring have chirality, therefore there are two enantiomters for NNN tools, i.e., (S)-NNN
(R)-NNN.Toxicologic study prove (S)-NNN carcinogenicity be better than (R)-NNN.Therefore, for NNN enantiomerisms in tobacco
The separation of body and measurement can provide potential reference for smoking and the relevant research of health, or reduction cigarette endangers Journal of Sex Research and carries
For potential new approaches.
Document report at present about NNN stage enantiomer separations is less, and only Hecht S.S. seminars reported two kinds
Analysis method.One kind analyzing joint technology based on gas-chromatography-thermal energy, and the process employs Cyclosil-B chiral columns, analyses
Time is longer, in about 35min (S)-NNN and (R)-NNN just detaches completely.Another kind is to be based on liquid chromatography-tandem mass spectrometry
Technology, this method is chiral stationary phase using 1 Kromasil of Pirkle Covalent (S, S)-Whelk-O, in about 22min
Inside realize (S)-NNN and (R)-NNN separation.And about (S)-NNN and (R)-NNN separation conjunction phase chromatography or close phase chromatography
Tandem mass spectrometry has not been reported.Phase chromatographic tandem mass spectrum is closed its essence is a kind of chromatographic technique based on supercritical fluid chromatography,
In recent years, with major improvement on supercritical fluid chromatograph device so that it has wider application space, also results in more
Carry out the concern of more researchers.Nontoxic, nonflammable and free from environmental pollution shooting flow is equally used in view of phase chromatography is closed
Body CO2It is a kind of real green environmental protection technique as main mobile phase, has compared to liquid chromatogram and gas-chromatography many prominent
Go out advantage, there is good separating degree and selectivity for analogue, isomers, enantiomer and diastereoisomer, and
In conjunction with the use of tandem mass spectrum detector so that the sensitivity of detection further increases.
The characteristics of the present invention is directed to according to tobacco sample, by closing phase chromatographic tandem mass spectrography in tobacco sampleNIt is sub-
Nitro nornicotine（NNN）Optical isomer (S)-NNN and (R)-NNN carries out separation analysis and quantitative detection, method is quickly and spirit
Sensitivity is high, will be (S)-NNN and (R) measurement of-NNN provides potential high-throughput detection technique and support.
Invention content
The object of the present invention is to provide in a kind of tobacco sample (S)-NNN and (R)-NNN measure conjunction phase chromatographic tandem matter
Spectrum（UPC2-MSMS）Rapid analysis method extracts the NNN in tobacco sample using acidified methanol solution, extracting solution warp
After organic phase filter membrane filtering, UPC is used2- MSMS in extracting solution (S)-NNN and (R)-NNN carries out separation and quantitative detection.
The sample pre-treatments of this method are simple and environmentally-friendly and analysis time is short, suitable for tobacco (S)-NNN and (R)-NNN detection.
The purpose of the present invention is achieved through the following technical solutions：
In tobacco (S)-NNN and (R)-NNN assay method, include the following steps：
（1）0.25 ~ 0.5g offal samples are weighed, 5 ~ 10mL is added and contains 0.5%（v/v）The methanol solution of acetic acid, mistake after ultrasonic extraction
Filter, obtains solution to be measured；
（2）It takes solution to be measured to carry out ultra high efficiency and closes phase chromatographic tandem mass spectrum（UPC2-MS/MS）Analysis, analysis condition are as follows：
Chromatographic condition：Using CHIRALPAK IG-3 chromatographic columns, specification 100mm × 3.0mm, 3.0 μm, column temperature：35℃；
Sample size：1μL；Mobile phase A：CO2, Mobile phase B：Methanol；Flow velocity：1.5mL/min；Back pressure：2000psi；Compensate solvent：Contain
0.1%（v/v）The methanol solution of formic acid, flow velocity：0.3mL/min；Gradient is as shown in table 1.
Mass Spectrometry Conditions：Electric spray ion source（ESI）, positive ion mode, source temperature：150°C；Capillary voltage：4.5kV；
Remove solvent temperature degree：350℃；Go solvent stream fast：800 L/h；Blowback gas velocity：50L/h；Multiple-reaction monitoring pattern（MRM）,
Detail parameters are shown in Table 2.
。
（3）Quantitatively calculated in sample using external standard calibration curve method (S)-NNN and (R)-NNN content.
Step（1）The power of middle ultrasonic extraction is 100W, frequency 40KHz, 30 ~ 60min of extraction time.
Step（1）Middle filtering uses 0.22 μm of organic phase filter membrane.
Step（3）Middle external standard calibration curve method is：Prepare containing (S)-NNN and (R)-NNN objects series standard work
Solution carries out regression analysis to its concentration with the chromatographic peak area of object, obtains standard curve；By step（2）Analysis knot
Fruit substitutes into standard curve, obtains the concentration of object in solution to be measured；Be calculated in sample again (S)-NNN and (R)-NNN
Content.
Beneficial effects of the present invention
The present invention establishes in tobacco for the first timeNNitrosonornicotine（NNN）Optical isomer (S)-NNN and (R)-NNN separation and
The conjunction phase chromatographic tandem mass spectrometry method of measurement.Mainly according to tobacco sample the characteristics of, to influencing the chromatography of chromatographic isolation effect
The selection of column is optimized.The sample pretreatment process of this method is simple, quick, is convenient for the analysis of batch sample.And with
When conjunction phase chromatographic tandem mass spectrum is detected, used main mobile phase is supercritical fluid CO2, cosolvent use minute quantity
Methanol, have the advantages that environmental-friendly.This detection method to (S) detection of-NNN is limited to 0.21ng/mL, quantitatively it is limited to
0.69ng/mL, to (R) detection of-NNN is limited to 0.34ng/mL, quantitatively it is limited to 1.12ng/mL.This method high sensitivity repeats
Property is good, suitable for tobacco sampleNThe separation of nitrosonornicotine optical isomer and measurement.
Description of the drawings
Fig. 1 is to select different chromatographic column separating effect comparison diagrams.
Fig. 2 is sample extracting solution total ion current figure.
Specific implementation mode
Present invention combination example is described further, but is not intended to limit the present invention.
Example 1：
（1）Instrument and reagent：
Close phase chromatographic tandem mass spectrograph（Waters, US）；Ultrasound Instrument（KQ-700DB types, the limited public affairs of city of Kunshan's ultrasonic instrument
Department）.
Racemic NNN and (R)-NNN standard items（Canadian Toronto Research Chemicals）；Methanol（South Korea
DUKSAN, chromatographically pure）；Acetic acid（>=99.7%, Fisher Scientific）.
（2）Instrument operating condition：
The chromatographic condition and Mass Spectrometry Conditions of instrument are as previously described, are not repeated herein.
Wherein, in chromatographic condition the selection of chromatographic column mainly investigated CHIRALPAK AD-3 chromatographic columns and
CHIRALPAK IG-3 chromatographic columns.In different chromatographic columns (S)-NNN and (R)-NNN separating resulting it is as shown in Figure 1.It can
See, in view of close phase chromatography excellent separative efficiency, (S)-NNN and (R)-NNN is split into two colors in two kinds of chromatographic columns
Spectral peak, this is by-the N in NNN=OEWithZAlloisomerism generation (E)-NNN and (Z)-NNN.Therefore racemic NNN standards
Product are split into 4 chromatographic peaks on chiral column.When previous literature report detects NNN in LC-MSMS methods, due toEWithZIt is three-dimensional different
The presence of structure and there is acromion phenomenon, and UPC2The result for almost reaching baseline separation that-MS/MS is obtained is equal in previous research
It has not been reported.
In addition, it should be noted that by (R)-NNN standard items analysis it is found that in CHIRALPAK AD-3 colors
Compose column on, chromatographic peak 1 and 3 it is corresponding be (S)-NNNEWithZStereoisomer, 2 and 4 it is corresponding be (R)-NNNEWithZIt is vertical
Body isomers.And in CHIRALPAK IG-3 chromatographic columns, chromatographic peak 1 and 2 it is corresponding be (S)-NNNEWithZAlloisomerism
Body, 3 and 4 it is corresponding be (R)-NNNEWithZStereoisomer.In view of we need concern (S)-NNN and (R)-NNN group
At without paying close attention in each optical isomerEWithZStereomeric composition, and in view of convenient for instrument automatic integration and
Quantitative, final determine uses CHIRALPAK IG-3 chromatographic columns.
（3）Sample pre-treatments：
Weigh 0.5g（It is accurate to 0.0001g）For offal sample in the conical flask with stopper of 50mL, the accurate 10mL that is added contains 0.5% vinegar
Triangular flask is covered rear 100W ultrasonic extractions 60min by sour methanol solution.Extracting solution is filtered with 0.22 μm of water phase filter membrane
To solution to be measured, using UPC2- MSMS is measured.
（4）Standard working solution is prepared：
The preparation of standard working solution includes mainly preparation and the racemic NNN series standard works of racemic NNN standard reserving solutions
Make the preparation of solution, specific process for preparation is as follows：
Racemic NNN primary standard storing solutions：Mass concentration is prepared by solvent of methanol as the racemic NNN level-one marks of 1mg/mL
Quasi- storing solution.
Racemic NNN secondary standard storing solutions：The accurate 0.1mL racemics NNN primary standards storing solution that pipettes holds in 10mL
In measuring bottle, with methanol constant volume to scale, the racemic NNN two level list mark storing solutions that concentration is respectively 100 μ g/mL are obtained.
Series standard working solution：Respectively pipette 20 μ L, 40 μ L, 100 μ L, 200 μ L, 400 μ L, 1000 μ L100 μ g/mL it is outer
Racemization NNN two levels list mark storing solution, with methanol constant volume to scale, it is molten to obtain series standard work in different 10mL volumetric flasks
Liquid, the wherein concentration of NNN are respectively 20ng/mL, 40ng/mL, 100ng/mL, 200ng/mL, 400ng/mL, 1000ng/mL, phase
Answer (S)-NNN and (R)-NNN concentration be 10ng/mL, 20ng/mL, 50ng/mL, 100ng/mL, 200ng/mL,
500ng/mL
（5）Sample measures
By step（4）Gained series standard working solution carries out UPC2- MS/MS is analyzed, with the quota ion chromatographic peak of object
Area（A）To its concentration（C）Regression analysis is carried out, standard curve is obtained.By step（3）Gained sample filtrate carries out UPC2-MS/
MS is analyzed, and the total ion current figure of acquired sample solution is as shown in Figure 2.Analysis result is substituted into standard curve, is obtained to be measured
The concentration of object in solution, then pass through formula（1）Be calculated in sample (S)-NNN and (R)-NNN content.
Wherein,X i For in tobacco sample (S)-NNN and (R)-NNN content, unit be μ g/g；C i To be calculated by graticule
To sample conjecture solution in (S)-NNN and (R)-NNN content, unit ng/mL；V is the volume of sample extracting solution,
10mL；m i For the tobacco sample quality weighed, 0.5g.
According to minimum primary standard working solution, respectively with the detection of 3 times of signal-to-noise ratio and 10 times of signal-to-noise ratio computation this method
Limit and quantitative limit.The results are shown in Table 3 for the range of linearity, linear equation, detection limit and quantitative limit of this method.
Be calculated in burley tobaccos sample according to standard working curve (S)-NNN and (R)-NNN three times parallel determination concentration with
And it is scaled to content in sample the results are shown in Table 4.
。
Claims (5)
1. in growing tobaccoNNitrosonornicotine（NNN）The conjunction phase chromatographic tandem mass spectrum side that optical isomer is detached and measured
Method, it is characterised in that：Include the following steps：
（1）0.25 ~ 0.5g offal samples are weighed, the methanol solution that 5 ~ 10mL contains 0.5% acetic acid is added, filters, obtains after ultrasonic extraction
To solution to be measured；
（2）It takes solution to be measured to carry out ultra high efficiency and closes phase chromatographic tandem mass spectrum（UPC2-MS/MS）Analysis, analysis condition are as follows：
Chromatographic condition：Using CHIRALPAK IG-3 chromatographic columns, specification 100mm × 3.0mm, 3.0 μm, column temperature：35℃；
Sample size：1μL；Mobile phase A：CO2, Mobile phase B：Methanol；Flow velocity：1.5mL/min；Back pressure：2000psi；Compensate solvent：Contain
The methanol solution of 0.1% formic acid；Flow velocity：0.3mL/min；Gradient is as shown in table 1：
Mass Spectrometry Conditions：Electric spray ion source（ESI）, positive ion mode, source temperature：150°C；Capillary voltage：4.5kV；It goes molten
Agent temperature degree：350℃；Go solvent stream fast：800 L/h；Blowback gas velocity：50L/h；Multiple-reaction monitoring pattern（MRM）, in detail
Parameter is shown in Table 2：
（3）Quantitatively calculated in sample using external standard calibration curve method (S)-NNN and (R)-NNN content.
2. according to the method described in claim 1, it is characterized in that：Step（1）The power of middle ultrasonic extraction is 100W, and frequency is
40KHz, 30 ~ 60min of extraction time.
3. according to the method described in claim 1, it is characterized in that：Step（1）Middle filtering uses 0.22 μm of organic phase filter membrane.
4. according to the method described in claim 1, it is characterized in that：Step（3）Middle external standard calibration curve method is：Prepare containing (S)-
NNN and (R)-NNN objects series standard working solution, with the chromatographic peak area of object to its concentration carry out return point
Analysis, obtains standard curve；By step（2）Analysis result substitute into standard curve in, obtain the concentration of object in solution to be measured；
Be calculated in sample again (S)-NNN and (R)-NNN content.
5. according to the method described in claim 1, it is characterized in that：Distinguish in the concentration of series standard working solution, wherein NNN
For 20ng/mL, 40ng/mL, 100ng/mL, 200ng/mL, 400ng/mL, 1000ng/mL, corresponding (S)-NNN and (R)-NNN
Concentration be 10ng/mL, 20ng/mL, 50ng/mL, 100ng/mL, 200ng/mL, 500ng/mL.
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Cited By (5)
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| CN111983109A (en) * | 2020-09-03 | 2020-11-24 | 国家烟草质量监督检验中心 | Chiral analysis method of alkaloid in tobacco or tobacco product |
| CN111983108A (en) * | 2020-09-03 | 2020-11-24 | 国家烟草质量监督检验中心 | Chiral analysis method for main alkaloids in electronic smoke sol |
| CN111983110A (en) * | 2020-09-03 | 2020-11-24 | 国家烟草质量监督检验中心 | Chiral analysis method for nicotine and main metabolites thereof in blood plasma |
| CN113341015A (en) * | 2021-06-04 | 2021-09-03 | 国家烟草质量监督检验中心 | Method for determining triazole fungicide in plant-derived food |
| CN115015407A (en) * | 2022-05-19 | 2022-09-06 | 国家烟草质量监督检验中心 | Method for determining paraben isomer in essence |
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| CN111983109A (en) * | 2020-09-03 | 2020-11-24 | 国家烟草质量监督检验中心 | Chiral analysis method of alkaloid in tobacco or tobacco product |
| CN111983108A (en) * | 2020-09-03 | 2020-11-24 | 国家烟草质量监督检验中心 | Chiral analysis method for main alkaloids in electronic smoke sol |
| CN111983110A (en) * | 2020-09-03 | 2020-11-24 | 国家烟草质量监督检验中心 | Chiral analysis method for nicotine and main metabolites thereof in blood plasma |
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| CN111983108B (en) * | 2020-09-03 | 2022-07-12 | 国家烟草质量监督检验中心 | Chiral analysis method for main alkaloids in electronic smoke sol |
| CN111983110B (en) * | 2020-09-03 | 2022-07-12 | 国家烟草质量监督检验中心 | Chiral analysis method for nicotine and main metabolites thereof in blood plasma |
| CN113341015A (en) * | 2021-06-04 | 2021-09-03 | 国家烟草质量监督检验中心 | Method for determining triazole fungicide in plant-derived food |
| CN113341015B (en) * | 2021-06-04 | 2023-09-22 | 国家烟草质量监督检验中心 | Method for determining triazole fungicide in plant-derived food |
| CN115015407A (en) * | 2022-05-19 | 2022-09-06 | 国家烟草质量监督检验中心 | Method for determining paraben isomer in essence |
| CN115015407B (en) * | 2022-05-19 | 2024-01-19 | 国家烟草质量监督检验中心 | Method for determining parahydroxybenzoate isomer in essence |
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