CN103149295A - Method for simultaneously determining nitrate and nitrite in tobacco - Google Patents
Method for simultaneously determining nitrate and nitrite in tobacco Download PDFInfo
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- CN103149295A CN103149295A CN2013100607240A CN201310060724A CN103149295A CN 103149295 A CN103149295 A CN 103149295A CN 2013100607240 A CN2013100607240 A CN 2013100607240A CN 201310060724 A CN201310060724 A CN 201310060724A CN 103149295 A CN103149295 A CN 103149295A
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Abstract
The invention discloses a method for simultaneously determining nitrate and nitrite in tobacco, and the method comprises a sample pretreatment step and a detection step, wherein the sample pretreatment step is as follows: measuring a certain amount of samples, and utilizing water or dilute alkali as extraction reagent to extract nitrate and nitrite in the sample; and the detection step is as follows: adopting alkaline solution as leacheate after the extraction, adopting an anion-exchange column to separate, finally utilizing an electrically-conductive detector to detect, adopting a retention time to determine the quality, and adopting an external reference method to determine the quantity. The extraction reagent used in the method is environment-friendly and safe, an ultrasonic extraction way is simple to operate and high in efficiency; by adopting the anion-exchange column, nitrate and nitrite can be simultaneously separated and determined; a matrix of the electrically-conductive detector is small, and the sensitivity is high; the method is applicable to samples of different types such as flue-cured tobaccos, burley tobaccos, aromatic tobaccos, sheets, expanded tobaccos, cut stems, mixed cigarettes and flue-cured-type cigarettes; and the requirement for rapidly extracting, separating and determining nitrate and nitrite in tobacco and tobacco products in one step can be met.
Description
Technical field
The present invention relates to a kind of method of measuring objectionable impurities in tobacco, refer to especially a kind of method of measuring simultaneously nitrate and nitrite in tobacco.
Background technology
Nitrate and nitrite are the important nitrogen-containing compounds of a class in tobacco, and what of its content not only directly affect the jealous and quality of tobacco leaf, also can affect formation and the content of other nitrogen-containing compounds.Wherein, nitrite is the direct precursor thing of tobacco-specific nitrosamine especially, and its content is significantly relevant to the content of tobacco-specific nitrosamine.Along with the growing interest of people to tobacco-specific nitrosamine, how rapidly and accurately nitrate and nitrite are carried out the quantitative test ever more important that also seems.
At present, the method that is applicable to measure nitrate and nitrite is both at home and abroad mainly divided the three major types such as spectroscopic methodology, chromatography, electrochemical process are arranged, the method of sample pre-treatments also mainly concentrates on the fields such as water body, food, vegetables, has no report and be suitable for the tobacco sample pre-treatment with method for measuring simultaneously.Therefore be badly in need of groping and setting up mutually deserved detection method, to guarantee carrying out smoothly of tobacco safety evaluatio and harm reduction work.
Summary of the invention
For the weak point that present technology exists, the invention provides a kind of method of measuring simultaneously nitrate and nitrite in tobacco.When having solved in tobacco nitrate and nitrite, the method measures problem, filled up the technological gap that in the tobacco, nitrate and nitrite are measured simultaneously, and the sample preparation process is simple, sample stability good, detection limit is low, good reproducibility, sample recovery rate are high, is suitable for extensive popularization.
In order to solve the problems of the technologies described above, the present invention adopts following technical scheme:
A kind of method of measuring simultaneously nitrate and nitrite in tobacco, the method comprises sample pre-treatments and detecting step; Described sample pre-treatments step is to take a certain amount of sample, nitrate and nitrite take water or diluted alkaline as extraction agent in the extraction sample; Described detecting step is: after extraction, take alkaline solution as leacheate, adopt anion-exchange column to separate, detect with electric conductivity detector at last, qualitative with retention time, external standard method is quantitative.
Furtherly, the method for sample pre-treatments is: take 0.5～1.5g sample in the 250mL conical flask, accurately add 50～100mL water or 50～100mL to contain OH
-At 1mmol to the M between 100mmol (OH)
nAqueous solution as extraction agent, cover plug and be placed on the ultrasonic or oscillator of ultrasonic cleaning machine vibration 30～120min, standing after, get supernatant liquor and namely get extract after 0.45 μ m water membrane filtration.
Furtherly, described water is ultrapure water, intermediate water or distilled water.
Furtherly, sample detection step: get the 4mL extract and pack in the 5mL sample injection bottle, through wearing peace AS40 injector sample introduction, (4mm * 250mm, band AS11-HG guard column 4mm * 50mm) are analytical column, M (OH) to wear peace IonPac AS11 chromatographic column
nAqueous solution be that the eluent gradient wash-out separates, the AS-4mm electric conductivity detector detects.
Furtherly, described M (OH)
nAqueous solution in M be that Na, karat gold belong to.
The usefulness of technique scheme is:
It is extractant that the present invention adopts water or diluted alkaline, not only environmental protection but also safety; Take ultrasonic as the extraction mode, simple to operate, efficient is high; Adopt anion-exchange column, separation determination when realizing nitrate and nitrite; The employing electric conductivity detector is measured, and matrix is little, highly sensitive; The method universality is strong, is applicable to the dissimilar samples such as flue-cured tobacco, burley tobaccos, Turkish tobaccos, thin slice, expanded cut tobacco, stem, blended type cigarette, Virginian-type cigarette; Can satisfy the requirement of the disposable Rapid Extraction separation determination of nitrate and nitrite in tobacco and goods thereof.
Description of drawings
Fig. 1 is the chromatographic fractionation figure of sample solution in the embodiment of the present invention 1.
Embodiment
Further set forth the present invention below in conjunction with specific embodiment.These embodiment only are not used in for explanation the present invention and limit the scope of the invention.
A kind of method of measuring simultaneously nitrate and nitrite in tobacco, the method comprises sample pre-treatments and detecting step; Described sample pre-treatments step is to take a certain amount of sample, nitrate and nitrite take water or diluted alkaline as extraction agent in the extraction sample; Described detecting step is: after extraction, take alkaline solution as leacheate, adopt anion-exchange column to separate, detect with electric conductivity detector at last, qualitative with retention time, external standard method is quantitative.
The preferred embodiment of the present invention is as follows:
Embodiment 1:
Sample pre-treatments: take 0.5g(and be accurate to 0.1mg) sample in the 250mL conical flask, accurately adds 50mL water as extraction agent, and described water can be ultrapure water, intermediate water or distilled water.Cover plug and be placed on the ultrasonic 60min of ultrasonic cleaning machine.After standing, get supernatant liquor and namely get extract through 0.45 μ m water membrane filtration.
Sample detection step: get the 4mL extract and pack in the 5mL sample injection bottle; through wearing peace AS40 injector sample introduction; to wear peace IonPac AS11 chromatographic column (4mm * 250mm; band AS11-HG guard column 4mm * 50mm) is separating column; the aqueous solution of KOH is mobile phase; flow velocity 1.2mL/min, rejector electric current 179MA adopts the AS-4mm electric conductivity detector to detect.Wherein elution program is: it is constant that the concentration of 0 minute to the 6th minute KOH is preserved 5mmol/L, concentration from the 6.1st minute to the 20th minute KOH changes to 10mmol/L by the 5mmol/L alternation, sport 60mmol/L and remain to the 25th minute since the concentration of the 20.1st minute KOH, sport 5mmol/L and remain to the 30th minute since the concentration of the 25.1st minute KOH.
Testing result: the chromatogram of sample extraction liquid as shown in Figure 1, NO
2 -And NO
3 -Flowed out at the 11.5th minute and 21.3 minutes respectively, peak shape is good, has no Interference Peaks.This elution program adopted low concentration KOH solution leacheate in from 0 to 20 minute, to guarantee NO
2 -And NO
3 -Separation be not subjected to the interference of other quasi-molecular ions; Then improve the KOH solution concentration to 60mmol/L, accelerate wash-out CO
3 2-, SO
4 2-In the ion of multivalent ion and some difficult wash-outs to avoid the pollution of coupled columns; Then reduce the KOH solution concentration, make the balance of pillar, for next sample is prepared; Whole gradient process only needs 30 minutes.
Embodiment 2:
The part tobacco sample is detected.
Sample pre-treatments: with tobacco sample balance 48h under 22 ℃ ± 1 ℃ and relative humidity 60% ± 2% condition, taking 0.8g(and be accurate to 0.1mg) sample is in the 250mL conical flask, accurately add aqueous solution that 75mL contains 10mmol/L KOH as extraction agent, cover plug and be placed on the ultrasonic 90min of ultrasonic cleaning machine.After standing, get supernatant liquor and namely get extract through 0.45 μ m water membrane filtration.
Sample detection step: get the 4mL extract and pack in the 5mL sample injection bottle; through wearing peace AS40 injector sample introduction; to wear peace IonPac AS11 chromatographic column (4mm * 250mm; band AS11-HG guard column 4mm * 50mm) is separating column; the aqueous solution of NaOH is mobile phase; flow velocity 1.0mL/min, rejector electric current 160MA adopts the AS-4mm electric conductivity detector to detect.Wherein elution program is: it is constant that the concentration of 0 minute to the 5th minute NaOH is preserved 6mmol/L, concentration from the 5.1st minute to the 18th minute NaOH changes to 12mmol/L by the 6mmol/L alternation, sport 80mmol/L and remain to the 22nd minute since the concentration of the 18.1st minute NaOH, sport 5mmol/L and remain to the 25th minute since the concentration of the 22.1st minute NaOH.
Typical curve: accurately take respectively 0.06g sodium nitrite, 1.37g sodium nitrate, be accurate to 0.1mg, the water dissolving, constant volume is 1000mL, namely is mixed with NO
2 -, NO
3 -Concentration is respectively the storing solution of 40mg/L, 1000mg/L.Be formulated as follows the working curve of concentration range: c (NO
2 -): 0.040,0.100,0.200,0.400,0.800,1.600mg/L; C (NO
3 -): 1.000,2.500,5.000,10.000,20.000,40.000mg/L.The accurate working solution of label taking carries out ion chromatography respectively, according to concentration and the response peak area of standard operation solution, Criterion working curve, working curve linearly dependent coefficient R
2Should be not less than 0.999.
Result is calculated: NO in sample
2 -, NO
3 -Content (X) calculated by formula (1), result represents with mg/kg:
In formula: X---NO in sample
2 -, NO
3 -Content, unit be the milligram every kilogram (mg/kg); C---the NO that is drawn by standard working curve
2 -, NO
3 -Concentration, unit is every liter (mg/L) of milligram; c
o---NO in the blank that drawn by standard working curve
2 -, NO
3 -Concentration, unit is every liter (mg/L) of milligram; V---sample extract constant volume, unit is milliliter (mL); The quality of m---sample, unit is gram (g); W---the massfraction of sample moisture, %.
Testing result: result is as shown in table 1: NO in tobacco leaf
2 -Content little, between 8.29～35.46mg/kg, dissimilar sample difference is less; NO
3 -Differ greatly in dissimilar sample, between 31.11～19151.42mg/kg, content roughly rule is: burley tobaccos〉stem〉Turkish tobaccos〉reconstituted tobacco〉flue-cured tobacco.
Table 1 sample detection data (mg/kg)
Embodiment 3:
The part cigarette sample is detected.
Sample pre-treatments: with tobacco sample balance 48h under 22 ℃ ± 1 ℃ and relative humidity 60% ± 2% condition, taking 1.0g(and be accurate to 0.1mg) sample is in the 250mL conical flask, accurately add aqueous solution that 100mL contains 5mmol/L NaOH as extraction agent, cover plug and be placed on oscillator vibration 120min.After standing, get supernatant liquor and namely get extract through 0.45 μ m water membrane filtration.
Sample detection step: get the 4mL extract and pack in the 5mL sample injection bottle; through wearing peace AS40 injector sample introduction; to wear peace IonPac AS11 chromatographic column (4mm * 250mm; band AS11-HG guard column 4mm * 50mm) is separating column; the aqueous solution of KOH is mobile phase; flow velocity 0.8mL/min, rejector electric current 200MA adopts the AS-4mm electric conductivity detector to detect.。Wherein elution program is: it is constant that the concentration of 0 minute to the 7th minute KOH is preserved 8mmol/L, concentration from the 7.1st minute to the 22nd minute KOH changes to 15mmol/L by the 8mmol/L alternation, sport 100mmol/L and remain to the 25th minute since the concentration of the 22.1st minute KOH, sport 5mmol/L and remain to the 28th minute since the concentration of the 25.1st minute KOH.
Typical curve: accurately take respectively 0.06g sodium nitrite, 1.37g sodium nitrate, be accurate to 0.1mg, the water dissolving, constant volume is 1000mL, namely is mixed with NO
2 -, NO
3 -Concentration is respectively the storing solution of 40mg/L, 1000mg/L.Be formulated as follows the working curve of concentration range: c (NO
2 -): 0.032,0.040,0.100,0.200,0.400,0.800mg/L; C (NO
3 -): 0.800,1.000,2.500,5.000,10.000,20.000mg/L.The accurate working solution of label taking carries out ion chromatography respectively, according to concentration and the response peak area of standard operation solution, Criterion working curve, working curve linearly dependent coefficient R
2Should be not less than 0.999.
Result is calculated: NO in sample
2 -, NO
3 -Content (X) calculated by formula (1), result represents with mg/kg:
In formula: X---NO in sample
2 -, NO
3 -Content, unit be the milligram every kilogram (mg/kg); C---the NO that is drawn by standard working curve
2 -, NO
3 -Concentration, unit is every liter (mg/L) of milligram; c
o---NO in the blank that drawn by standard working curve
2 -, NO
3 -Concentration, unit is every liter (mg/L) of milligram; V---sample extract constant volume, unit is milliliter (mL); The quality of m---sample, unit is gram (g); W---the massfraction of sample moisture, %.
Testing result: result is as shown in table 2: NO
2 -Content little, between 8.45～30.09mg/kg, dissimilar sample difference is less; NO
3 -Differ greatly in dissimilar sample, between 185.20～10808.13mg/kg, content roughly rule is: blended type cigarette〉Virginian-type cigarette.
Table 12 sample detection data (mg/kg)
Above-mentioned is only three specific embodiments of the present invention, but design concept of the present invention is not limited to this, allly utilizes this design to carry out the change of unsubstantiality to the present invention, all should belong to the behavior of invading protection domain of the present invention.
Claims (6)
1. method of measuring simultaneously nitrate and nitrite in tobacco, it is characterized in that: the method comprises sample pre-treatments and detecting step; Described sample pre-treatments step is to take a certain amount of sample, nitrate and nitrite take water or diluted alkaline as extraction agent in the extraction sample; Described detecting step is: after extraction, take alkaline solution as leacheate, adopt anion-exchange column to separate, detect with electric conductivity detector at last, qualitative with retention time, external standard method is quantitative.
2. a kind of method of measuring simultaneously nitrate and nitrite in tobacco as claimed in claim 1, it is characterized in that: the method for described sample pre-treatments is: take 0.5～1.5g sample in the 250mL conical flask, accurately add 50～100mL water or 50～100mL to contain OH
-At 1mmol to the M between 100mmol (OH)
nAqueous solution as extraction agent, cover plug and be placed on the ultrasonic or oscillator of ultrasonic cleaning machine vibration 30～120min, standing after, get supernatant liquor and namely get extract after 0.45 μ m water membrane filtration.
3. a kind of method of measuring simultaneously nitrate and nitrite in tobacco as claimed in claim 2, it is characterized in that: described water is ultrapure water, intermediate water or distilled water.
4. as claim 1,2 or 3 a kind of described methods of measuring simultaneously nitrate and nitrite in tobacco; it is characterized in that: the sample detection step: get the 4mL extract and pack in the 5mL sample injection bottle; through wearing peace AS40 injector sample introduction; to wear peace IonPac AS11 chromatographic column (4mm * 250mm; band AS11-HG guard column 4mm * 50mm) is analytical column, M (OH)
nAqueous solution be that the eluent gradient wash-out separates, the AS-4mm electric conductivity detector detects.
5. a kind of method of measuring simultaneously nitrate and nitrite in tobacco as claimed in claim 2 or claim 3, is characterized in that: described M (OH)
nAqueous solution in M be that Na, karat gold belong to.
6. a kind of method of measuring simultaneously nitrate and nitrite in tobacco as claimed in claim 4, is characterized in that: described M (OH)
nAqueous solution in M be that Na, karat gold belong to.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112730664A (en) * | 2020-12-22 | 2021-04-30 | 贵州省烟草科学研究院 | Method for measuring nitrate and nitrite in fresh tobacco leaves by combining heat extraction with dispersed solid phase extraction |
| CN114894925A (en) * | 2022-04-26 | 2022-08-12 | 中国神华煤制油化工有限公司 | Method for measuring oxalic acid content in dimethyl oxalate |
| WO2023206109A1 (en) * | 2022-04-26 | 2023-11-02 | 中国神华煤制油化工有限公司 | Method for determining oxalic acid content of dimethyl oxalate |
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| CN102128885A (en) * | 2010-12-08 | 2011-07-20 | 广东中烟工业有限责任公司 | Method for quickly and simultaneously detecting 16 inorganic anions and organic acids in tobacco |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN102128885A (en) * | 2010-12-08 | 2011-07-20 | 广东中烟工业有限责任公司 | Method for quickly and simultaneously detecting 16 inorganic anions and organic acids in tobacco |
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| 吴玉萍等: "梯度淋洗离子色谱法测定烟草中的苹果酸、柠檬酸和阴离子", 《分析试验室》 * |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112730664A (en) * | 2020-12-22 | 2021-04-30 | 贵州省烟草科学研究院 | Method for measuring nitrate and nitrite in fresh tobacco leaves by combining heat extraction with dispersed solid phase extraction |
| CN114894925A (en) * | 2022-04-26 | 2022-08-12 | 中国神华煤制油化工有限公司 | Method for measuring oxalic acid content in dimethyl oxalate |
| WO2023206109A1 (en) * | 2022-04-26 | 2023-11-02 | 中国神华煤制油化工有限公司 | Method for determining oxalic acid content of dimethyl oxalate |
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Application publication date: 20130612 |