CN105699503A - Method for simultaneously determining content of sodium, potassium, magnesium and calcium in tobaccos - Google Patents
Method for simultaneously determining content of sodium, potassium, magnesium and calcium in tobaccos Download PDFInfo
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- CN105699503A CN105699503A CN201610025065.0A CN201610025065A CN105699503A CN 105699503 A CN105699503 A CN 105699503A CN 201610025065 A CN201610025065 A CN 201610025065A CN 105699503 A CN105699503 A CN 105699503A
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- G01N30/02—Column chromatography
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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
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- G01N30/64—Electrical detectors
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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
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- G01N2030/645—Electrical detectors electrical conductivity detectors
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Abstract
The invention discloses a method for simultaneously determining the content of sodium, potassium, magnesium and calcium in tobaccos. The method includes the concrete operation steps that after being ground and screened, a tobacco sample is extracted in a vortex mode with a hydrochloric acid aqueous solution, an extracting solution is subjected to diluting, volume setting and filtering and analyzed through an ion chromatography-electrical conductivity detector, and therefore the content of sodium, potassium, magnesium and calcium in tobaccos can be determined simultaneously through one-time sample introduction. The method is short in analysis time, high in sensitivity and repeatability, large in recovery rate and capable of fast, accurately and quantitatively analyzing the content of sodium, potassium, magnesium and calcium in tobaccos in batches, and pretreatment is easy to operate.
Description
Technical field
The invention belongs to technical field of analysis and detection, particularly relate to a kind of method of sodium, potassium, magnesium, calcium content in Nicotiana tabacum L. of mensuration simultaneously。
Background technology
Sodium in Nicotiana tabacum L., potassium, magnesium, calcium content cigarette quality is had material impact, wherein potassium, calcium, magnesium are the three big mineral elements that content in Nicotiana tabacum L. is maximum。Potash fertilizer can improve leaf color, identity, flammability and hygroscopicity, and the quality of tobacco that potassium content is higher is better；Potassium to the flammability of Nicotiana tabacum L., glow and hold firepower and hygroscopicity plays an important role。Magnesium can make burning after ash be not easily scattered, and high its ash color of Nicotiana tabacum L. of magnesium content is general more gloomy, and the quality of cigar is particularly had certain effect by Medicated cigarette by this。Calcium is the basis of cell wall structure, and calcium content is similar to potassium or slightly above potassium, is conducive to improving the filling capacity of Nicotiana tabacum L.。In addition, sodium, potassium can increase Medicated cigarette and hold firepower, plays combustion-supporting effect；Magnesium, calcium are the ash elements that Nicotiana tabacum L. is important。For sodium, potassium, magnesium, calcium catalyst in Nicotiana tabacum L., the standard that tobacco business has been promulgated has YC/T174 2003 " Nicotiana tabacum L. and tobacco product calcium catalyst atomic absorption method ", YC/T173 2003 " the mensuration flame spectrometry of Nicotiana tabacum L. and tobacco product potassium ", YC/T217 2007 " the mensuration continuous flow method of Nicotiana tabacum L. and tobacco product potassium ", YC/T175 2003 " the mensuration atomic absorption method of Nicotiana tabacum L. and tobacco product magnesium "。The detector of above-mentioned several method is atomic absorption spectrum and ultraviolet spectrophotometer, and the range of linearity is narrow, poor anti jamming capability, can not realize analyzing while sodium, potassium, magnesium, 4 kinds of components of calcium。Adopting ICP MS to measure the report of 27 kinds of mineral elements in Nicotiana tabacum L. additionally, also have, the sample pre-treatments of ICP MS method needs to use concentrated hydrochloric acid micro-wave digestion, and ICP MS operating cost is high。
In recent years, the chromatography of ions because of sample pre-treatments and instrumentation is simple, operating cost is low, highly sensitive, analysis time is short, can analyze the advantages such as different kinds of ions simultaneously become measure anions and canons prefered method。Having been reported that the sodium adopted in ion-chromatographic determination Nicotiana tabacum L., potassium, magnesium, calcium at present, pretreatment mode has the extraction of homogenate method, ultrasonic extraction, wet digesting, dry ashing etc.。The acid concentration of wet digesting use is too high, and the post effect of cation analysis post is had considerable influence；Dry ashing complex operation, consuming time longer。At present without sodium in extraction of ocean eddies Simultaneous Determination Nicotiana tabacum L., potassium, magnesium, the square patent of calcium content and bibliographical information。
Summary of the invention
It is an object of the invention to provide a kind of method adopting ion chromatograph simultaneously to measure sodium in Nicotiana tabacum L., potassium, magnesium, calcium content, the method is easy and simple to handle, fast, highly sensitive, accuracy of analyzing speed and sensitivity good, it is adaptable to the quick mensuration of sodium, potassium, magnesium, calcium content in high-volume tobacco sample。
For achieving the above object, the present invention takes techniques below scheme:
A kind of method of sodium, potassium, magnesium, calcium content in Nicotiana tabacum L. of mensuration simultaneously, comprises the following steps:
Step one, uses the mixed standard solution of hydrochloric acid solution preparation sodium, potassium, magnesium, calcium, carries out ion chromatography, draw the standard working curve of sodium, potassium, magnesium, calcium；
Step 2, after tobacco sample is ground, sieved, measures moisture content, obtains ground sample；
Step 3, joins ground sample in hydrochloric acid solution, carries out extraction of ocean eddies on vortex instrument；Then centrifugal on centrifuge, take supernatant dilution constant volume, filtration, obtain sample to be analyzed；
Step 4, adopts ion chromatography to measure the concentration of the sodium in sample to be analyzed, potassium, magnesium, calcium, calculates and obtain sodium in Nicotiana tabacum L., potassium, magnesium, calcium content。
Further improve, in described step one, draw the standard working curve of sodium, potassium, magnesium, calcium method particularly includes:
First prepare the sodium of 100 μ g/mL, potassium, magnesium, calcium hybrid standard storing solution by secondary deionized water；Accurately pipette 0.1mL, 0.2mL, 0.5mL, 1mL, 2mL hybrid standard storing solution more respectively, be settled in 10mL volumetric flask with the hydrochloric acid solution of 35mmol/L, carry out ion chromatography, draw the standard working curve of sodium, potassium, magnesium, calcium。
Further improving, in described step 3, concentration of hydrochloric acid solution is 1mol/L, and hydrochloric acid solution volume is 20～30mL；When the rotating speed of extraction of ocean eddies is 1000～2000r/min, the extraction of ocean eddies time is 5～20min；Centrifugal rotational speed is 10000～15000r/min, and centrifugation time is 10～20min；0.22 μm of aqueous phase filter membrane is used during filtration。
Further improving, step one and in step 4, ion chromatography condition is as follows:
Ion chromatograph model: ThermoFisherICS2100；
Chromatographic column: DionexIonPacCS16,4mm × 250mm；
Guard column: DionexIonPacCG16,4mm × 50mm；
Suppressor model: DionexCERS 500, it is suppressed that device electric current: 103mA；
Leacheate: methanesulfonic acid, concentration: 25～35mmol/L；
Leacheate flow velocity: 1.0～1.5mL/min, isocratic elution；
Sample size: 10～25 μ L；
Column temperature: 40 DEG C；
Electric conductivity detector；
Chi Wen: 45 DEG C。
Further improving, described tobacco sample is flue-cured tobacco, burley tobaccos, Turkish tobaccos, reconstituted tobacco, blended type cigarette or Virginian-type cigarette。
The invention has the beneficial effects as follows: adopt hydrochloric acid solution to extract sodium, potassium, magnesium, calcium in Nicotiana tabacum L., with CS16 ion exchange column, sodium, potassium, magnesium, calcium in Nicotiana tabacum L. are easily separated, ion chromatography electric conductivity detector is adopted to detect, realize single injected sampling, measure the content of sodium, potassium, magnesium, calcium in Nicotiana tabacum L. simultaneously。The invention provides a kind of easy and simple to handle, analyze that speed is fast, highly sensitive, accuracy and reproducible measure the method for sodium, potassium, magnesium, calcium content in Nicotiana tabacum L., it is adaptable to high-volume tobacco sample quickly analyze mensuration。
Accompanying drawing explanation
Sodium that Fig. 1 present invention obtains, potassium, magnesium, calcium mixed standard solution chromatogram；
The chromatogram of sodium, potassium, magnesium, calcium in the typical sample that Fig. 2 present invention obtains。
Detailed description of the invention
Following implementation process and embodiment are further intended to the present invention is described and should not be construed as limitation of the invention。
1, the instrument of the present invention and reagent, material
ThermoFisherICS2100 ion chromatograph；Vortex instrument；High speed centrifuge；50mL centrifuge tube；10mL centrifuge tube；Hydrochloric acid；Sodium, potassium, magnesium, calcium standard solution, medium is water, and concentration is 1000mg/L；Secondary deionized water。
2, tobacco sample pre-treatment:
After tobacco sample is ground, sieves (40 order), measure moisture content, obtain ground sample；Weigh ground sample 0.5000g in 50mL centrifuge tube, add the hydrochloric acid solution of 25mL1mol/L, rotating speed extraction of ocean eddies 20min with 2000r/min, then about 5mL extracting solution is taken in 10mL centrifuge tube, with the centrifugal 15min of the rotating speed of 10000r/min, supernatant after centrifugal, through 0.22 μm of aqueous phase membrane filtration, enters ion chromatography。3, ion chromatography condition:
Ion exchange column: DionexIonPacCS16 post (4mm × 250mm)；Guard column is DionexIonPacCG16 (50mm × 4mm)；Leacheate: methanesulfonic acid, flow velocity is 1.0mL/min；Column temperature: 40 DEG C；Pond temperature 45 DEG C；Suppressor electric current 103mA；Sample size 25 μ L。Adopt qualitative with standard sample contrast retention time, quantified by external standard method。The chromatogram of standard specimen as it is shown in figure 1, the chromatogram of sample as shown in Figure 2。
4, working curve and detection limit, quantitative limit:
First prepare the sodium of 100 μ g/mL, potassium, magnesium, calcium hybrid standard storing solution by secondary deionized water；Accurately pipette 0.1mL, 0.2mL, 0.5mL, 1mL, 2mL hybrid standard storing solution more respectively, it is settled in 10mL volumetric flask with the hydrochloric acid solution of 35mmol/L, makes the standard working solution of 1 μ g/mL, 2 μ g/mL, 5 μ g/mL, 10 μ g/mL, 20 μ g/mL。Being measured by aforesaid ion chromatography condition, with peak area μ S value for vertical coordinate, with standard working solution concentration (μ g/mL) value for abscissa drawing curve, equation of linear regression, detection limit and quantitative limit are in Table 1。
Table 1 equation of linear regression, detection limit and quantitative limit
5, sodium in tobacco sample, potassium, magnesium, calcium content computing formula as follows:
Wherein c: Na, K, Mg, Ca measured value in sample, is drawn by standard working curve, unit micrograms per millilitre (μ g/mL)；
c0: blank Na, K, Mg, Ca measured value, standard working curve draw, unit micrograms per millilitre (μ g/mL)；
V: extracting liquid volume, unit is milliliter (mL)；
M: sample weighting amount, unit is gram (g)；
W: the percentage composition of moisture in sample, % (mass fraction)；
The extension rate of extracting solution。
For flue-cured tobacco sample, replication 6 times, calculating the relative standard deviation (RSD) of this method, and carry out recovery of standard addition experiment again according to sodium, potassium, magnesium, calcium content 1 in this sample, result is in Table 2。As seen from the results in Table 2, sodium, potassium, magnesium, calcium RSD respectively 4.47%, 1.68%, 3.62%, 3.88%, all within 5%, it was shown that the method repeatability of the present invention is very well；Sodium, potassium, magnesium, calcium the response rate respectively 90.56%, 95.74%, 93.57%, 92.86%, it was shown that this method is quantitatively accurate, meets the quantitative analysis requirement of sodium in Nicotiana tabacum L., potassium, magnesium, calcium。
Table 2 certain tobacco sample repeatability and response rate experimental result (n=6)
The method adopting the present invention determines the sodium in 8 tobacco samples, potassium, magnesium, calcium content, and result is in Table 3。
Na, K, Mg, Ca content (representing with %) in table 3 tobacco sample
Claims (8)
1. measure a method for sodium, potassium, magnesium, calcium content in Nicotiana tabacum L. simultaneously, comprise the following steps:
Step one, uses the mixed standard solution of hydrochloric acid solution preparation sodium, potassium, magnesium, calcium, carries out ion chromatography, draw the standard working curve of sodium, potassium, magnesium, calcium；
Step 2, after tobacco sample is ground, sieved, measures moisture content, obtains ground sample；
Step 3, joins ground sample in hydrochloric acid solution, carries out extraction of ocean eddies on vortex instrument；Then centrifugal on centrifuge, take supernatant dilution constant volume, filtration, obtain sample to be analyzed；
Step 4, adopts ion chromatography to measure the concentration of the sodium in sample to be analyzed, potassium, magnesium, calcium, calculates and obtain sodium in Nicotiana tabacum L., potassium, magnesium, calcium content。
2. the method for sodium, potassium, magnesium, calcium content in a kind of Nicotiana tabacum L. of mensuration simultaneously according to claim 1, it is characterised in that: in described step one, draw the standard working curve of sodium, potassium, magnesium, calcium method particularly includes:
First prepare the sodium of 100 μ g/mL, potassium, magnesium, calcium hybrid standard storing solution by secondary deionized water；Accurately pipette 0.1mL, 0.2mL, 0.5mL, 1mL, 2mL hybrid standard storing solution more respectively, be settled in 10mL volumetric flask with the hydrochloric acid solution of 35mmol/L, carry out ion chromatography, draw the standard working curve of sodium, potassium, magnesium, calcium。
3. the method for sodium, potassium, magnesium, calcium content in a kind of Nicotiana tabacum L. of mensuration simultaneously according to claim 1, it is characterised in that: in described step 3, concentration of hydrochloric acid solution is 1mol/L, and hydrochloric acid solution volume is 20～30mL；When the rotating speed of extraction of ocean eddies is 1000～2000r/min, the extraction of ocean eddies time is 5～20min；Centrifugal rotational speed is 10000～15000r/min, and centrifugation time is 10～20min；0.22 μm of aqueous phase filter membrane is used during filtration。
4. the method for sodium, potassium, magnesium, calcium content in a kind of Nicotiana tabacum L. of mensuration simultaneously according to claim 1, it is characterised in that: in described step one and step 4, ion chromatography condition is as follows:
Ion chromatograph model: ThermoFisherICS2100；
Chromatographic column: DionexIonPacCS16,4mm × 250mm；
Guard column: DionexIonPacCG16,4mm × 50mm；
Suppressor model: DionexCERS 500, it is suppressed that device electric current: 103mA；
Leacheate: methanesulfonic acid, concentration: 25～35mmol/L；
Leacheate flow velocity: 1.0～1.5mL/min, isocratic elution；
Sample size: 10～25 μ L；
Column temperature: 40 DEG C；
Electric conductivity detector；
Chi Wen: 45 DEG C。
5. the method for sodium, potassium, magnesium, calcium content in a kind of Nicotiana tabacum L. of mensuration simultaneously according to claim 1, it is characterised in that: in described step one, draw the standard working curve of sodium, potassium, magnesium, calcium method particularly includes:
First prepare the sodium of 100 μ g/mL, potassium, magnesium, calcium hybrid standard storing solution by secondary deionized water；Accurately pipette 0.1mL, 0.2mL, 0.5mL, 1mL, 2mL hybrid standard storing solution more respectively, be settled in 10mL volumetric flask with the hydrochloric acid solution of 35mmol/L, carry out ion chromatography, draw the standard working curve of sodium, potassium, magnesium, calcium；
In described step 3, concentration of hydrochloric acid solution is 1mol/L, and hydrochloric acid solution volume is 20～30mL；When the rotating speed of extraction of ocean eddies is 1000～2000r/min, the extraction of ocean eddies time is 5～20min；Centrifugal rotational speed is 10000～15000r/min, and centrifugation time is 10～20min；0.22 μm of aqueous phase filter membrane is used during filtration；
In described step one and step 4, ion chromatography condition is as follows:
Ion chromatograph model: ThermoFisherICS2100；
Chromatographic column: DionexIonPacCS16,4mm × 250mm；
Guard column: DionexIonPacCG16,4mm × 50mm；
Suppressor model: DionexCERS 500, it is suppressed that device electric current: 103mA；
Leacheate: methanesulfonic acid, concentration: 25～35mmol/L；
Leacheate flow velocity: 1.0～1.5mL/min, isocratic elution；
Sample size: 10～25 μ L；
Column temperature: 40 DEG C；
Electric conductivity detector；
Chi Wen: 45 DEG C。
6. according to the method for sodium, potassium, magnesium, calcium content in described a kind of Nicotiana tabacum L. of mensuration simultaneously arbitrary in claim 15, it is characterised in that: tobacco sample described in step 2 is flue-cured tobacco, burley tobaccos, Turkish tobaccos, reconstituted tobacco, blended type cigarette or Virginian-type cigarette。
7. according to the method for sodium, potassium, magnesium, calcium content in described a kind of Nicotiana tabacum L. of mensuration simultaneously arbitrary in claim 15, it is characterised in that: sieve described in step 2 as crossing 40 mesh sieves。
8. the method for sodium, potassium, magnesium, calcium content in a kind of Nicotiana tabacum L. of mensuration simultaneously according to claim 1, it is characterised in that: in described step one, draw the standard working curve of sodium, potassium, magnesium, calcium method particularly includes:
First prepare the sodium of 100 μ g/mL, potassium, magnesium, calcium hybrid standard storing solution by secondary deionized water；Accurately pipette 0.1mL, 0.2mL, 0.5mL, 1mL, 2mL hybrid standard storing solution more respectively, be settled in 10mL volumetric flask with the hydrochloric acid solution of 35mmol/L, carry out ion chromatography, draw the standard working curve of sodium, potassium, magnesium, calcium；
Tobacco sample described in step 2 is flue-cured tobacco, burley tobaccos, Turkish tobaccos, reconstituted tobacco, blended type cigarette or Virginian-type cigarette；Sieve described in step 2 as crossing 40 mesh sieves；
In described step 3, concentration of hydrochloric acid solution is 1mol/L, and hydrochloric acid solution volume is 20～30mL；When the rotating speed of extraction of ocean eddies is 1000～2000r/min, the extraction of ocean eddies time is 5～20min；Centrifugal rotational speed is 10000～15000r/min, and centrifugation time is 10～20min；0.22 μm of aqueous phase filter membrane is used during filtration；
In described step one and step 4, ion chromatography condition is as follows:
Ion chromatograph model: ThermoFisherICS2100；
Chromatographic column: DionexIonPacCS16,4mm × 250mm；
Guard column: DionexIonPacCG16,4mm × 50mm；
Suppressor model: DionexCERS 500, it is suppressed that device electric current: 103mA；
Leacheate: methanesulfonic acid, concentration: 25～35mmol/L；
Leacheate flow velocity: 1.0～1.5mL/min, isocratic elution；
Sample size: 10～25 μ L；
Column temperature: 40 DEG C；
Electric conductivity detector；
Chi Wen: 45 DEG C；
In described step 3, concentration of hydrochloric acid solution is 1mol/L, and hydrochloric acid solution volume is 20～30mL；When the rotating speed of extraction of ocean eddies is 1000～2000r/min, the extraction of ocean eddies time is 5～20min；Centrifugal rotational speed is 10000～15000r/min, and centrifugation time is 10～20min；0.22 μm of aqueous phase filter membrane is used during filtration；
In described step one and step 4, ion chromatography condition is as follows:
Ion chromatograph model: ThermoFisherICS2100；
Chromatographic column: DionexIonPacCS16,4mm × 250mm；
Guard column: DionexIonPacCG16,4mm × 50mm；
Suppressor model: DionexCERS 500, it is suppressed that device electric current: 103mA；
Leacheate: methanesulfonic acid, concentration: 25～35mmol/L；
Leacheate flow velocity: 1.0～1.5mL/min, isocratic elution；
Sample size: 10～25 μ L；
Column temperature: 40 DEG C；
Electric conductivity detector；
Chi Wen: 45 DEG C。
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Cited By (8)
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| CN106226455A (en) * | 2016-08-17 | 2016-12-14 | 广西中烟工业有限责任公司 | Ammonium, potassium, calcium and the analysis method of magnesium in a kind of Nicotiana tabacum L. of mensuration simultaneously |
| CN106872597A (en) * | 2017-02-28 | 2017-06-20 | 云南省烟草质量监督检测站 | The content assaying method of various cations in a kind of cigarette mainstream flue gas |
| CN106908564A (en) * | 2017-02-28 | 2017-06-30 | 云南省烟草质量监督检测站 | Lithium, sodium, ammonia, potassium, magnesium, the method for calcium content in smoke-free tobacco product are determined simultaneously |
| CN108845044A (en) * | 2018-05-03 | 2018-11-20 | 山东滨州智源生物科技有限公司 | The detection method of sodium content in a kind of sulfobutyl ether betadex sodium |
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| CN106226455A (en) * | 2016-08-17 | 2016-12-14 | 广西中烟工业有限责任公司 | Ammonium, potassium, calcium and the analysis method of magnesium in a kind of Nicotiana tabacum L. of mensuration simultaneously |
| CN106872597A (en) * | 2017-02-28 | 2017-06-20 | 云南省烟草质量监督检测站 | The content assaying method of various cations in a kind of cigarette mainstream flue gas |
| CN106908564A (en) * | 2017-02-28 | 2017-06-30 | 云南省烟草质量监督检测站 | Lithium, sodium, ammonia, potassium, magnesium, the method for calcium content in smoke-free tobacco product are determined simultaneously |
| CN106908564B (en) * | 2017-02-28 | 2019-04-05 | 云南省烟草质量监督检测站 | The method for measuring lithium in smoke-free tobacco product, sodium, ammonia, potassium, magnesium, calcium content simultaneously |
| CN106872597B (en) * | 2017-02-28 | 2019-10-25 | 云南省烟草质量监督检测站 | The content assaying method of a variety of cations in a kind of cigarette mainstream flue gas |
| CN108845044A (en) * | 2018-05-03 | 2018-11-20 | 山东滨州智源生物科技有限公司 | The detection method of sodium content in a kind of sulfobutyl ether betadex sodium |
| CN109142450A (en) * | 2018-07-17 | 2019-01-04 | 青岛大学 | Method based on electrical conductivity method measurement sugar alcohol fertilizer of chelated calcium chelation percent |
| CN109001340A (en) * | 2018-09-28 | 2018-12-14 | 湖北远大天天明制药有限公司 | A kind of rapid assay methods of low concentration salt flushing liquor multicomponent content |
| CN109507314A (en) * | 2018-10-29 | 2019-03-22 | 中科谱研（北京）科技有限公司 | The ion chromatography method of sodium, potassium, magnesium, calcium in Amino Acid Compound Injection |
| 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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Application publication date: 20160622 |