CN106226455A - Ammonium, potassium, calcium and the analysis method of magnesium in a kind of Nicotiana tabacum L. of mensuration simultaneously - Google Patents
Ammonium, potassium, calcium and the analysis method of magnesium in a kind of Nicotiana tabacum L. of mensuration simultaneously Download PDFInfo
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Abstract
The present patent application discloses one and measures ammonium in Nicotiana tabacum L., potassium, calcium and 4 kinds of cation analysis methods of magnesium simultaneously, said method comprising the steps of: 1) prepared by sample；2) sample extraction and process；3) preparation of standard working solution；4) ion chromatographic separation analysis.It is an advantage of the current invention that: could cover compared with these several important Nicotiana tabacum L. cationes with existing multiple methods, the present invention uses a method to extract and measure while achieving ammonium in Nicotiana tabacum L., potassium, calcium and 4 kinds of cationes of magnesium, and method pre-treatment is simple, reproducible, it is adaptable to the analysis of batch samples.
Description
Technical field
The invention belongs to Tobacco Analysis technical field, specifically a kind of use chromatography of ions measure simultaneously ammonium in Nicotiana tabacum L., potassium,
Calcium and 4 kinds of cation analysis methods of magnesium.
Technical background
In Nicotiana tabacum L., ammonium is released during Nicotiana tabacum L. burns and sucks and is free in flue gas, changes flue gas acid-base balance, thus
Change the jealous feature of flue gas, strong harsh feeling and zest can be brought during excessive concentration, make the suction taste of Nicotiana tabacum L. be deteriorated.Nicotiana tabacum L.
In potassium, calcium and magnesium be that tobacco growing grows necessary nutrient, potassium can improve the resistance against diseases of cigarette strain, and magnesium is plant
Metabolism plays an important role, and calcium is conducive to the maturation of cigarette strain.Potassium, calcium and magnesium have weight for result of combustion of tobacco performance simultaneously
Affect.Therefore, ammonium in Nicotiana tabacum L., potassium, calcium, magnesium are the important indicators of quality of tobacco evaluation and control.
At present, the ammonium in mensuration tobacco sample, potassium, calcium, magnesium are respectively adopted different methods.The mensuration of ammonium has colour developing-company
Continuous flow method, the chromatography of ions etc..Potassium, calcium, the mensuration of magnesium are mainly Atomic Absorption Spectrometer method and inductively coupled plasma
Mass spectrometry.Atomic Absorption Spectrometer method and icp ms method are not appropriate for the mensuration of ammonium ion, and show
Color-continuous flow method measures potassium, calcium, the magnesium needs independent method for building up of each index.Under existing method system, measure Nicotiana tabacum L. simultaneously
Middle ammonium, potassium, calcium, magnesium need different sample treatment and instrumental method, are unfavorable for improving work efficiency.Therefore, the present invention uses
Chromatography of ions, as detecting instrument, develops a kind of ammonium, potassium, calcium, the method for magnesium in Nicotiana tabacum L. of mensuration simultaneously.
Summary of the invention
It is an object of the invention to need multiple methods to carry out covering for ammonium in conventional Tobacco Analysis, potassium, calcium, magnesium and can not
The one simultaneously measured and provide is based on assay method while chromatography of ions.
The one that the present invention provides measures ammonium in Nicotiana tabacum L., potassium, calcium and 4 kinds of cation analysis methods of magnesium simultaneously, and it includes
Following steps:
1) prepared by sample:
Take tobacco sample to be detected, use baking oven to be dried；Dried sample is pulverized, and after pulverizing, sample sieves；
2) sample extraction and process:
Weigh a certain amount of 1) in preparation tobacco powder sample be placed in conical flask, add dilute hydrochloric acid, mechanical oscillation or
After sonic oscillation, take extraction solution through aqueous phase filtering with microporous membrane, obtain sample solution；
3) preparation of standard working solution；
4) ion chromatographic separation analysis:
By 2) in the solution that obtains carry out ion chromatography, ion chromatographic column is cation-exchange chromatography post.
Ammonium, potassium, calcium and the preferred side of 4 kinds of cation analysis methods of magnesium in a kind of Nicotiana tabacum L. of mensuration simultaneously that the present invention provides
Case is:
1) prepared by sample
Choose tobacco sample to be detected, use baking oven to be dried between 40～60 DEG C to moisture less than 10%.It is dried
Rear sample is pulverized, and after pulverizing, sample uses and sieves more than or equal to the dusting cover of 30 mesh.
2) sample extraction and process
Weigh the 0.1～0.5g tobacco powder sample prepared to be placed in conical flask, be quantitatively adding 100mL concentration be 0.1～
0.2mol/L dilute hydrochloric acid, is carried out after mechanical oscillation or sonic oscillation 1 hour, takes extraction solution micro-through 0.22 μm or 0.45 μm aqueous phase
Hole membrane filtration, obtains sample solution.
3) preparation of standard working solution: pipette a certain amount of ammonium respectively, potassium, calcium, the standard solution of magnesium are configured to series
Standard working solution, wherein ammonium concentration is respectively 0.1,0.5,2.0,5.0,10.0 μ g/mL, and potassium concn is respectively 10, and 20,50,
100,200 μ g/mL, calcium concentration is respectively 5,10,20,50,100 μ g/mL, and magnesium density is respectively 0.5, and 2.0,5.0,10.0,
20.0μg/mL。
4) ion chromatographic separation analysis
By 2) in the solution that obtains carry out ion chromatography, ion chromatographic column is CS-12A type cation exchange column, rule
Lattice are 250 × 4mm, and are configured with CG-12A type guard column, and specification is 50 × 4mm；Flowing is 0.02mol/L pyrovinic acid water mutually
Solution；Flow velocity: 1.0mL/min；Sample size is 25 μ L；It is 30 DEG C that column temperature controls.
In above-mentioned condition, carrying out sieving and use dilute hydrochloric acid extraction more than or equal to the dusting cover of 30 mesh by sample warp is we
The key of method, thinner sample particle is conducive to improving the extraction efficiency of ammonium, potassium, calcium, magnesium, and dilute hydrochloric acid is for ammonium, potassium, calcium, magnesium
Etc. cation, there is stronger solvability.
It is an advantage of the present invention that and could cover with existing multiple methods compared with these several important Nicotiana tabacum L. cationes, this
A kind of method of bright employing is extracted and is measured while achieving ammonium in Nicotiana tabacum L., potassium, calcium and 4 kinds of cationes of magnesium, and method pre-treatment
Simply, reproducible, it is adaptable to the analysis of batch samples.
Accompanying drawing explanation
Fig. 1 is the chromatogram using the inventive method to obtain, and wherein 1 is ammonium ion, and 2 is potassium ion, and 3 is magnesium ion, and 4 are
Calcium ion.
Specific embodiments
The present invention is described further below in conjunction with instantiation, but is not limiting as the present invention.
Fig. 1 is the chromatogram using the inventive method to obtain, and wherein 1 is ammonium ion, and 2 is potassium ion, and 3 is magnesium ion, and 4 are
Calcium ion.
Example 1
Choose He Nanxiang county 2015 and produce C3F grade flue-cured tobacco sample per year, use 40 DEG C of baking oven to be dried 6 hours, measure moisture
Value is 7.6%.Dried sample is pulverized, and uses the dusting cover of 30 mesh to sieve.Weigh tobacco powder prepared by 0.1g
End sample is placed in 150mL conical flask, is quantitatively adding the dilute hydrochloric acid that 100mL concentration is 0.1M, carries out mechanical oscillation 1 hour, take
Extraction solution, through 0.22 μm aqueous phase filtering with microporous membrane, obtains sample solution.The solution obtained is carried out ion chromatography, surveys
Determine the content of ammonium in solution, potassium, calcium, magnesium.Being calculated ammonium content in this flue-cured tobacco sample is 112 μ g/g, and potassium content is 13.2mg/
G, calcium content is 29.1mg/g, and content of magnesium is 5.1mg/g.
Example 2
Choose enshi 2015 and produce C3 grade burley tobaccos sample per year, use 60 DEG C of baking oven to be dried 4 hours, measure moisture
Value is 5.9%.Dried sample is pulverized, and uses the dusting cover of 40 mesh to sieve.Weigh tobacco powder prepared by 0.2g
End sample is placed in 150mL conical flask, is quantitatively adding the dilute hydrochloric acid that 100mL concentration is 0.2M, carries out sonic oscillation 1 hour, take
Extraction solution, through 0.45 μm aqueous phase filtering with microporous membrane, obtains sample solution.The solution obtained is carried out ion chromatography, surveys
Determine the content of ammonium in solution, potassium, calcium, magnesium.Being calculated ammonium content in this sample is 3132 μ g/g, and potassium content is 21.9mg/g,
Calcium content is 24.1mg/g, and content of magnesium is 4.1mg/g.
Example 3
Pipette a certain amount of ammonium respectively, potassium, calcium, the standard solution of magnesium are configured to series standard working solution, and wherein ammonium is dense
Degree is respectively 0.1,0.5,2.0,5.0,10.0 μ g/mL, and potassium concn is respectively 10, and 20,50,100,200 μ g/mL, calcium concentration divides
Not being 5,10,20,50,100 μ g/mL, magnesium density is respectively 0.5,2.0,5.0,10.0,20.0 μ g/mL.With described in method from
Sub-chromatographic condition carries out ammonium, potassium, calcium, magnesium determination.Carry out linear regression according to concentration of standard solution and each peak area, obtain standard
Working curve and linearly dependent coefficient, with least concentration mixed standard solution continuous sample introduction 10 times, obtain the mark of ammonium, potassium, calcium, magnesium
Quasi-deviation, using 3 times of standard deviations as detection limit, using 10 times of standard deviations as quantitative limit.The detection limit of method and quantitative limit
It is shown in Table 1.
The detection limit of table 1 method and quantitative limit
Example 4
Select certain brand commercial cigarettes sample, after tobacco shred is taken out, use 60 DEG C of baking oven to be dried 4 hours, measure moisture
Value is 8.6%.Dried sample is pulverized, and uses the dusting cover of 40 mesh to sieve.Weigh tobacco shred powder prepared by 0.5g
End sample is placed in 150mL conical flask, is quantitatively adding the dilute hydrochloric acid that 100mL concentration is 0.15M, carries out mechanical oscillation 1 hour, take
Extraction solution, through 0.45 μm aqueous phase filtering with microporous membrane, obtains sample solution.The solution obtained is carried out ion chromatography, surveys
Determine the content of ammonium in solution, potassium, calcium, magnesium.Carry out 6 times to measure simultaneously, be calculated relative standard deviation, evaluate and obtain method essence
Density is between 2.6%～9.6%.
Table 2 method precision
Claims (8)
1. one kind measures ammonium, potassium, calcium and the analysis method of magnesium in Nicotiana tabacum L. simultaneously, it is characterised in that described method includes following step
Rapid:
1) prepared by sample:
Take tobacco sample to be detected, use baking oven to be dried；Dried sample is pulverized, and after pulverizing, sample sieves；
2) sample extraction and process:
Weigh a certain amount of 1) in preparation tobacco powder sample be placed in conical flask, add dilute hydrochloric acid, mechanical oscillation or ultrasonic
After vibration, take extraction solution through aqueous phase filtering with microporous membrane, obtain sample solution；
3) preparation of standard working solution；
4) ion chromatographic separation analysis:
By 2) in the solution that obtains carry out ion chromatography, ion chromatographic column is cation-exchange chromatography post.
Ammonium, potassium, calcium and the analysis method of magnesium in a kind of Nicotiana tabacum L. of mensuration simultaneously the most according to claim 1, it is characterised in that
Step 1) sample is prepared as:
Choose tobacco sample to be detected, use baking oven to be dried between 40～60 DEG C to moisture less than 10%；Dried sample
Product are pulverized, and after pulverizing, sample uses and sieves more than or equal to the dusting cover of 30 mesh.
Ammonium, potassium, calcium and the analysis method of magnesium in a kind of Nicotiana tabacum L. of mensuration simultaneously the most according to claim 1, it is characterised in that
Step 2) sample extraction and being processed as: weigh the 0.1～0.5g tobacco powder sample prepared and be placed in conical flask, be quantitatively adding
100mL concentration is 0.1～0.2mol/L dilute hydrochloric acid, carries out after mechanical oscillation or sonic oscillation 1 hour, takes extraction solution through 0.22
μm or 0.45 μm aqueous phase filtering with microporous membrane, obtain sample solution.
Ammonium, potassium, calcium and the analysis method of magnesium in a kind of Nicotiana tabacum L. of mensuration simultaneously the most according to claim 3, it is characterised in that
Step 2) in, microporous filter membrane is 0.22 μm.
Ammonium, potassium, calcium and the analysis method of magnesium in a kind of Nicotiana tabacum L. of mensuration simultaneously the most according to claim 1, it is characterised in that
Step 3) being formulated as of standard working solution: pipette a certain amount of ammonium respectively, potassium, calcium, the standard solution of magnesium are configured to series mark
Quasi-working solution, wherein ammonium concentration is respectively 0.1,0.5,2.0,5.0,10.0 μ g/mL, and potassium concn is respectively 10, and 20,50,
100,200 μ g/mL, calcium concentration is respectively 5,10,20,50,100 μ g/mL, and magnesium density is respectively 0.5, and 2.0,5.0,10.0,
20.0μg/mL。
Ammonium, potassium, calcium and the analysis method of magnesium in a kind of Nicotiana tabacum L. of mensuration simultaneously the most according to claim 1, it is characterised in that
Step 4) ion chromatographic separation analysis is: by 2) in the solution that obtains carry out ion chromatography, chromatographic column is CS-12A type sun
Ion exchange column, specification is 250 × 4mm, and is configured with CG-12A type guard column, and specification is 50 × 4mm；Flowing is mutually
0.02mol/L pyrovinic acid aqueous solution；Flow velocity: 1.0mL/min；Sample size is 25 μ L；Column temperature: 30 DEG C.
Ammonium, potassium, calcium and the analysis method of magnesium in a kind of Nicotiana tabacum L. of mensuration simultaneously the most according to claim 1, it is characterised in that
Said method comprising the steps of:
1) prepared by sample
Choose tobacco sample to be detected, use baking oven to be dried between 40～60 DEG C to moisture less than 10%；Dried sample
Product are pulverized, and after pulverizing, sample uses and sieves more than or equal to the dusting cover of 30 mesh；
2) sample extraction and process
Weigh the 0.1～0.5g tobacco powder sample prepared to be placed in conical flask, be quantitatively adding 100mL concentration be 0.1～
0.2mol/L dilute hydrochloric acid, is carried out after mechanical oscillation or sonic oscillation 1 hour, takes extraction solution micro-through 0.22 μm or 0.45 μm aqueous phase
Hole membrane filtration, obtains sample solution；
3) being formulated as of standard working solution: pipette a certain amount of ammonium respectively, potassium, calcium, the standard solution of magnesium are configured to series mark
Quasi-working solution, wherein ammonium concentration is respectively 0.1,0.5,2.0,5.0,10.0 μ g/mL, and potassium concn is respectively 10, and 20,50,
100,200 μ g/mL, calcium concentration is respectively 5,10,20,50,100 μ g/mL, and magnesium density is respectively 0.5, and 2.0,5.0,10.0,
20.0μg/mL；
4) ion chromatographic separation analysis
By 2) in the solution that obtains carry out ion chromatography, ion chromatographic column is CS-12A type cation exchange column, and specification is
250 × 4mm, and it is configured with CG-12A type guard column, specification is 50 × 4mm；Flowing is that 0.02mol/L pyrovinic acid is water-soluble mutually
Liquid；Flow velocity: 1.0mL/min；Sample size is 25 μ L；It is 30 DEG C that column temperature controls.
Ammonium, potassium, calcium and the analysis method of magnesium in a kind of Nicotiana tabacum L. of mensuration simultaneously the most according to claim 1, it is characterised in that:
Choose flue-cured tobacco sample, use 40 DEG C of baking oven to be dried 6 hours, measure moisture value less than 10%；Dried sample is pulverized,
And use the dusting cover of 30 mesh to sieve；
Weigh flue-cured tobacco powder sample prepared by 0.1g to be placed in 150mL conical flask, be quantitatively adding dilute salt that 100mL concentration is 0.1M
Acid, carries out mechanical oscillation 1 hour, take extraction solution through 0.22 μm aqueous phase filtering with microporous membrane, obtain sample solution；
Pipette a certain amount of ammonium respectively, potassium, calcium, the standard solution of magnesium are configured to series standard working solution, and wherein ammonium concentration divides
Not being 0.1,0.5,2.0,5.0,10.0 μ g/mL, potassium concn is respectively 10,20,50,100,200 μ g/mL, and calcium concentration is respectively
5,10,20,50,100 μ g/mL, magnesium density is respectively 0.5,2.0,5.0,10.0,20.0 μ g/mL；
The sample solution obtained is carried out ion chromatography, measures ammonium, potassium, calcium, the content of magnesium in solution.
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| CN106645503A (en) * | 2017-02-28 | 2017-05-10 | 云南省烟草质量监督检测站 | Measuring method of contents of Li<+>, Na<+>, NH4<+>, K<+>, Mg<2+> and Ca<2+> ions in smoke-laden packaging bag |
| CN108279280A (en) * | 2018-01-31 | 2018-07-13 | 安徽瑞思威尔科技有限公司 | A kind of effective method of potassium in quick detection pit mud |
| CN111707776A (en) * | 2020-04-30 | 2020-09-25 | 民丰特种纸股份有限公司 | Accurate detection method for citrate content in cigarette paper |
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| CN106645503A (en) * | 2017-02-28 | 2017-05-10 | 云南省烟草质量监督检测站 | Measuring method of contents of Li<+>, Na<+>, NH4<+>, K<+>, Mg<2+> and Ca<2+> ions in smoke-laden packaging bag |
| CN108279280A (en) * | 2018-01-31 | 2018-07-13 | 安徽瑞思威尔科技有限公司 | A kind of effective method of potassium in quick detection pit mud |
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