CN105372371B - Ion chromatographic method and the application of reconstituted tobacco oxalate, amber acid radical, sulfate radical and phosphate radical are determined simultaneously - Google Patents
Ion chromatographic method and the application of reconstituted tobacco oxalate, amber acid radical, sulfate radical and phosphate radical are determined simultaneously Download PDFInfo
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- CN105372371B CN105372371B CN201510870988.1A CN201510870988A CN105372371B CN 105372371 B CN105372371 B CN 105372371B CN 201510870988 A CN201510870988 A CN 201510870988A CN 105372371 B CN105372371 B CN 105372371B
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Abstract
The invention discloses a kind of while determine the ion chromatographic method of reconstituted tobacco oxalate, amber acid radical, sulfate radical and phosphate radical.The present invention establishes using pyrovinic acid as extract solution and ensures that the extraction efficiency of each component to be measured in sample reaches more than 99.7%, simultaneously using sodium carbonate and sodium acid carbonate mixed solution as mobile phase, effectively eliminate the ascorbate degradation influence quantitative to oxalate, sample treatment and sample introduction can detect reconstituted tobacco oxalate simultaneously, amber acid radical, four kinds of components of sulfate radical and phosphate radical, the relative standard deviation of each component test content to be measured is 0.27%~0.99%, recovery of standard addition is between 99.3%~106.2%, accurately, simply, reliably, simultaneously suitable for tobacco sample and reconstituted tobacco sample related component measure.
Description
Technical field
The present invention relates to the detection technique field of reconstituted tobacco, is determined simultaneously in reconstituted tobacco more particularly, to a kind of
Oxalate, amber acid radical, sulfate radical and the chromatography of ions detection method of phosphate radical and application.
Background technology
Because it has balance tobacco structure, stable cigarette quality, effectively reduction tar and part have papermaking-method reconstituted tobaccos
Do harm to the advantage of composition burst size and more and more utilized., it is necessary to add various in papermaking-method reconstituted tobaccos process
Auxiliary agent, wherein butanedioic acid (succinic acid) and oxalic acid are added into as process assistant, phosphoric acid as extraction auxiliary agent.Based on reconstruction cigarette
Leaf product quality is stable and security consideration, the addition of each analog assistant will be controlled strictly, it is therefore desirable to establishes a set of accurate and effective
Method of testing in reconstituted tobacco auxiliary agent residual test.
The chromatography of ions (IC) is used widely with the characteristics of good, the high sensitivity of selectivity, pre-treatment is simple.Cigarette
The measure of anion, cation and organic acid uses the chromatography of ions more in grass and its product, but has no and have been reported that while determine
Reconstituted tobacco mesoxalic acid, butanedioic acid, the method for sulfate radical and phosphate content.There are many ion-chromatographic determinations to include cigarette at present
The grass plant containing vitamin C (ascorbic acid) and food mesoxalic acid content method, but document above does not account for tieing up inside
The influence that raw plain C determines to oxalic acid, the influence that vitamin C determines to oxalic acid is only considered in the detection of biological fluid medical science.Mesh
The method of preceding measure tobacco mesoxalic acid all has two：First, the incomplete of oxalic acid is extracted using pure water as extract；
Second, making leacheate using the stronger NaOH of alkalescence, vitamin C in tobacco (ascorbic acid) is caused to be converted into oxalic acid and make measure
As a result it is higher.
The content of the invention
The technical problem to be solved in the present invention is, for existing reconstituted tobacco oxalate, amber acid radical, sulfate radical and phosphorus
The deficiency of sour detection technique, reconstituted tobacco oxalate, amber acid radical, sulfate radical and phosphate radical can be determined simultaneously by establishing one kind
The ion chromatographic method of content, it is intended to which the control to chemical substance addition in reconstituted tobacco process provides technical basis.
Another technical problem to be solved by the present invention is that provide the application of the detection method.
The goal of the invention of the present invention is achieved by the following technical programs：
Chromatography of ions side that is a kind of while determining reconstituted tobacco oxalate, amber acid radical, sulfate radical and phosphate radical is provided
Method, by reconstituted tobacco sample using pyrovinic acid as extract oscillation extraction after through membrane filtration, then carry out chromatography of ions point
Analysis；
Chromatographiccondition, analytical column：AS22-4mm；Column temperature：30℃；Leacheate：4.5mmol/L NaCO3+
1.4mmol/L NaHCO3；Flow velocity：1.2mL/min；Sample size：50μL；Suppressor electric current： 31mA.Detector：Self-loopa is cloudy
Ion Suppressor conductivity detection.
Preferably, also include filtrate solid-phase extraction column purified treatment step before the ion chromatography.Due to again
Make tobacco leaf ingredient complexity, sample extraction liquid by purification remove may cause chromatographic column pollute macromolecular substances, then carry out from
Sub- chromatography.
Present invention preferably employs SPE RP posts effectively impurity screening composition and to have the higher pre-treatment rate of recovery.
Preferably, the flow velocity of filtrate described in purified treatment is 0.5mL/min.The RP posts use 5mL first respectively before using
Alcohol and 10ml pure water are activated with 1mL/min flow velocity.
Preferably, the concentration of the pyrovinic acid is 40mmol/L.
Preferably, the time of the oscillation extraction is 20~60 minutes, further preferred 30min.
Four kinds of objects to be measured are all water soluble anions, for chromatography of ions detect, conventional Extraction solvent be pure water,
Acid solution and sodium hydroxide solution.But exemplified by being extractant with pure water, it is to reconstituted tobacco sample and its once extracts
Experimental summary, the extraction efficiency of oxalic acid only have 37.7%, can not single extraction it is complete.The present invention can be very using 40mmol/L MSA
Good extracts four kinds of object ions, does not detect oxalic acid in extraction residue, extraction efficiency reaches 99.7% or more.
The present invention is by carefully studying summary, preferred analytical columns of the AS22 as this method, and four kinds of target components are at this
There is good separating effect on post；And the influence of flow rate of mobile phase and sample size is further compared, flow velocity 1.2mL/min,
Sample size is promoted into 50 μ L can significantly improve the sensitivity of composition to be measured, and sample introduction repeatability RSD reaches 0.13%~0.7%.
The inventive method can be advantageously applied to tobacco sample and reconstituted tobacco sample mesoxalic acid, butanedioic acid, sulfuric acid and/
Or the measure of the measure related component of phosphoric acid components；And all kinds of organic additive mesoxalic acids, amber suitable for reconstituted tobacco
The measure of acid, sulfuric acid and/or phosphoric acid components.
Beneficial effects of the present invention：
The present invention has filled up the blank of prior art, there is provided it is a kind of determine simultaneously reconstituted tobacco oxalate, amber acid radical,
The chromatography of ions detection method of sulfate radical and phosphate radical.Establish using sodium carbonate-bicarbonate mixed system as leacheate,
40mmol/L pyrovinic acids (MSA) are extract solution, AS22 be splitter IC determine reconstituted tobacco oxalate, amber acid radical,
The method of phosphate radical and sulfuric acid acid content.It this method solve using water as extract solution and leacheate measure oxalic acid content made with NaOH
Irrationality, make oxalate in sample quantitatively more accurate, reliable, moreover, applied to determining reconstituted tobacco simultaneously
When oxalate, amber acid radical, sulfate radical and phosphoric acid, the relative standard deviation (RSD) of each component test content to be measured is
0.27%~0.99%, recovery of standard addition is accurate, simple, reliable between 99.3%~106.2%, while is applied to tobacco
In sample and reconstituted tobacco sample the measure of related component and suitable for reconstituted tobacco all kinds of organic additives measure.
Brief description of the drawings
The lower separation spectrogram of vitamin C and oxalic acid standard liquid on AS18 posts of Fig. 1 various concentrations NaOH solution elution.
Wherein, spectrogram 1,3,5,7-vitamin C standard liquid；Spectrogram 2,4,6,8-oxalic acid standard liquid.
Fig. 2 vitamin Cs standard liquid produces oxalic acid content ratio under the conditions of different solvents matrix and various concentrations leacheate
Relatively result (ug/mL).
The extraction efficiency comparative result of Fig. 3 various concentrations pyrovinic acid extracts.
Fig. 4 difference extraction time test result comparative results (peak area).
Fig. 5 vitamin Cs are in 4.5mM NaCO3+1.4mM NaHCO3Chromatogram under leacheate.
Wherein, 1-vitamin C of spectrogram standard liquid；2-four kinds of desired anion mixed standard solutions of spectrogram.
Fig. 6 actual samples test chromatogram.
Embodiment
Below in conjunction with the accompanying drawings the present invention is further illustrated with specific embodiment.Following being given for example only property of embodiment explanations,
It is not considered as limiting the invention.Unless stated otherwise, the reagent used in following embodiments is conventional purchased in market or business
The reagent that approach obtains, unless stated otherwise, the method and apparatus used in following embodiments is side commonly used in the art
Method and equipment.
Materials and methods：
1.1 materials, reagent and instrument
The present invention illustrates by taking the 26 reconstituted tobacco trial targets and finished product that randomly select as an example；Aqueous phase filter membrane
(0.45um, wishing Podbielniak)；Solid phase extraction column (RP posts, 1cc, the U.S. wear peace)；(AS22-4mm, the U.S. are worn chromatographic column
Peace).
Pyrovinic acid (MSA) (99%, Fluka companies of the U.S.)；Natrium carbonicum calcinatum (benchmark product, Tianjin red rock chemical reagent work)；
Sodium carbonate (100%, pure chemical Analysis Co.Ltd)；Vitamin C (ascorbic acid) (99%, U.S. Sigma-
Aldrich)；Oxalic acid (99%, Acros companies of the U.S.)；Phosphate radical, sulfate radical standard liquid (1000ug/ml, country's mark
Quasi- material center)；Six water butanedioic acids (99%, Sigma-Aldrich)；Ultra-pure water (resistivity >=18.2M Ω
cm)。
ICS5000 ion chromatographs (Dai An companies of the U.S.)；Milli-Q ultra-pure water instrument (U.S. Millipore)；
CP224S electronic balances (sensibility reciprocal 0.0001g, German Sartorius companies)；HY-5 oscillators (domestic Jiangsu).
The influence experiment that the vitamin C of embodiment 1 determines to oxalate
Much include tobacco at present all makes in the chromatography of ions for including ascorbic plant oxalate assay
Oxalate and other anion are separated by the use of NaOH solution as leacheate.The study find that vitamin C can be converted at a high ph
Oxalic acid.100ug/ml vitamin C standard liquids are prepared by solvent of water, 10mmol/ is used respectively on AS18 anion analysis posts
L, 20mmol/L, 30mmol/LNaOH solution isocratic elution and the elution conduct of 11mmol/L~50mmol/LNaOH solution gradients
Mobile phase program, vitamin C standard liquid is determined, having oxalate appearance on test chromatogram, (retention time is qualitative, sees figure
Shown in 1).Fig. 2 is shown using the 100ug/mL vitamin C standard liquids prepared under two kinds of solvent substrates of pure water and pyrovinic acid
The amount of oxalic acid is produced when various concentrations NaOH solution elutes.Result above shows：About 50% vitamin C is converted into grass
Acid, therefore NaOH can not be used as extract solution and leacheate when measure contains ascorbic sample medium-height grass acid content, it is no
Then, test result oxalic acid content can be caused higher.
The research experiment of the sample-pretreating method of embodiment 2
Four kinds of objects to be measured are all water soluble anions, are detected for chromatography of ions, and conventional Extraction solvent is pure water,
Acid solution and sodium hydroxide solution.It can not be extracted due to described in embodiment 1 using strong alkali solution.Experiment is with pure water
Extractant extracted to reconstituted tobacco sample and its once after residue carry out 30 minutes concussion extraction, measure four kinds of targets into
Point.As a result show to use pure water that the extraction efficiency of oxalic acid only has 37.7% for extractant, can not single extraction it is complete.Due to this
Analytical column used in method is anion column, and conventional acid ion can bring anion to disturb, therefore experiment employs difference
Concentration pyrovinic acid (MSA) is extractant.As a result show (as shown in Figure 3)：It can be extracted well using 40mmol/L MSA
Go out four kinds of object ions, do not detect oxalic acid in extraction residue, extraction efficiency reaches 99.7%.
Using 40mmol/L MSA as extractant, influence of the different duration of oscillations to test result have studied, the results showed that
Four kinds of target component test results difference in 20~60 minutes duration of oscillations is little, comprehensive various factors, determines Best Times
For 30 minutes (as shown in Figure 4).
Due to reconstituted tobacco complicated component, sample extraction liquid, which needs to remove by purification, may cause the big of chromatographic column pollution
Molecular substance, then carry out ion chromatography.Experiment shows that SPE RP posts effectively impurity screening composition and can have higher
The pre-treatment rate of recovery.
The determination experiment of the chromatographic condition of embodiment 3
Studied for a long period of time experimental summary and previous reasons based on the present invention, it is impossible to using NaOH solution as leacheate, examination
Test to have inquired into and use NaCO3+NaHCO3Possibility as mobile phase, the results showed that (see Fig. 5), using 4.5mmol/L NaCO3
+1.4mmol/L NaHCO3Make leacheate, vitamin C standard liquid is not converted to oxalic acid.Study tour is more simultaneously for experiment
Kind chromatographic column, such as the chromatographic column such as AS14, AS22, are carried out from Multiple factors such as separating degree, peak shape symmetry, peak width and sensitivity
Comparative analysis, preferably determines analytical columns of the AS22 as this method, and four kinds of target components have good separation on the post；Compare
The influence of flow rate of mobile phase and sample size, flow velocity 1.2ml/min, sample size is promoted into 50 μ L can significantly improve butanedioic acid
Sensitivity, sample introduction repeatability RSD reaches 0.13%~0.7%.
The interfering ion development test of embodiment 4
The present invention has investigated the Common Anions such as fluorine in tobacco, chlorine, nitric acid, nitrite anions and formic acid, acetic acid, third simultaneously
The influences of the organic acid to experiment such as acid, lactic acid, malic acid, malonic acid and the distinctive fumaric acid of reconstituted tobacco.As a result show fluorine,
Chlorine, nitric acid, nitrite anions and formic acid, acetic acid, propionic acid, lactic acid all concentrate on appearance before 10min, malic acid, malonic acid and Fu Ma
Acid while the appearance among sulfate radical and amber acid radical, have good separation (as shown in Figure 6) with determinand.
Embodiment 5 determines working curve and detection limit
Use 40mmol/L MSA preparing standard solutions respectively, oxalate and succinate ion in four kinds of target components
The linear response under MSA matrix, but sulfate radical and phosphate radical then respond under MSA matrix for conic section.
1000ug/mL phosphate radical, sulfate radical, amber acid radical and oxalate standard reserving solution is used respectively, is configured to table 1
Series standard working solution, carry out ion chromatography.Concentration (X, the ug/ responsed to which with the peak area (Y) of object
ML) it is fitted recurrence.The standard liquid point of least concentration in series standard solution is taken, continuous sample introduction 10 times, calculates standard deviation
Poor (SD), the detection limit using 3 times of SD as method.Regression equation, coefficient correlation and detection limit are shown in Table 2.
The hybrid standard working solution concentration (ug/ml) of table 1
The regression equation of table 2, coefficient correlation and detection limit
The rate of recovery of embodiment 6 and Precision Experiment
Reconstituted tobacco sample accurately is weighed, is measured according to the inventive method, each sample is repeated 5 times, the results showed that
(shown in table 3), sample object component content relative standard deviation (RSD) are 0.27%~0.99%, the repeatability of illustration method
Preferably.The sample solution of known content is taken, the standard liquid for being separately added into three concentration levels carries out IC analysis, calculates recovery
Rate, as a result display is (shown in table 4), and the rate of recovery is between 99.3%~106.2%, and the degree of accuracy of illustration method is higher, Ke Yiman
The requirement of sufficient quantitative analysis.
The method reperformance test result (n=5) of table 3
The method recovery of standard addition of table 4
The sample pre-treatments of embodiment 7 and chromatography
Sample and determination sample moisture are prepared according to GB/T19616 and YC/T 31-1996, accurately weigh 0.1g samples
(being accurate to 0.0001g) adds 50.0mL40mmol/L MSA extracts, covers plug, put in 150mL ground triangular flasks
In on oscillator, oscillation extraction 30min.Sample solution is extracted with 0.5mL/min flow velocity through RP solid phases again through membrane filtration, filtrate
Take column purification (RP posts are activated with 5ml methanol and 10ml pure water with 1mL/min flow velocity respectively using preceding), finally carry out from
Sub- chromatography.
Chromatographiccondition, analytical column：AS22-4mm；Column temperature：30℃；Leacheate：4.5mmol/L NaCO3+
1.4mmol/L NaHCO3；Flow velocity：1.2mL/min；Sample size：50μL；Suppressor electric current： 31mA.Detector：Self-loopa is cloudy
Ion Suppressor conductivity detection.
Test agent in 26 reconstituted tobaccos randomly selected and tobacco finished product sample are measured using this method, as a result
It is shown in Table 5.MSA extract solutions may contain a small amount of sulfate radical and phosphate anion, enter line blank test deduction if necessary.This
Inventive method is simultaneously suitable for the measure of tobacco.
The actual sample of table 5 determines (mg/g)
The present invention is established using sodium carbonate-bicarbonate mixed system as leacheate, 40mmol/L pyrovinic acids (MSA)
For extract solution, AS22 is that the IC of splitter determines the side of reconstituted tobacco oxalate, amber acid radical, phosphate radical and sulfuric acid acid content
Method.The irrationality for making leacheate measure oxalic acid content using water as extract solution and with NaOH is this method solve, is made in sample
Oxalic acid is quantitatively more accurate, reliable, the measure of all kinds of organic additives suitable for reconstituted tobacco.
Claims (7)
1. ion chromatographic method that is a kind of while determining reconstituted tobacco oxalate, amber acid radical, sulfate radical and phosphate radical, it is special
Sign is, by reconstituted tobacco sample using pyrovinic acid as extract oscillation extraction after through membrane filtration, then carry out ion color
Spectrum analysis；
The chromatographiccondition, analytical column：AS22-4mm；Column temperature：30℃；Leacheate：4.5mmol/LNaCO3+1.4mmol/L
NaHCO3；Flow velocity：1.2mL/min；Sample size：50μL；Suppressor electric current：31mA；Detector：Self-loopa anion suppresses conductance
Detection；
The concentration of the pyrovinic acid is 40mmol/L；
Also include filtrate carrying out purified treatment step, the solid phase extraction using solid-phase extraction column before the ion chromatography
It is to use SPE RP posts to take column purification processing.
2. determine the ion of reconstituted tobacco oxalate, amber acid radical, sulfate radical and phosphate radical simultaneously according to claim 1
Chromatographic process, it is characterised in that the RP posts are carried out with 5mL methanol and 10ml pure water with 1mL/min flow velocity respectively before using
Activation.
3. determine the ion of reconstituted tobacco oxalate, amber acid radical, sulfate radical and phosphate radical simultaneously according to claim 1
Chromatographic process, it is characterised in that the flow velocity of filtrate described in the purified treatment is 0.5mL/min.
4. determine the ion of reconstituted tobacco oxalate, amber acid radical, sulfate radical and phosphate radical simultaneously according to claim 1
Chromatographic process, it is characterised in that the time of the oscillation extraction is 20~60 minutes.
5. determine the ion of reconstituted tobacco oxalate, amber acid radical, sulfate radical and phosphate radical simultaneously according to claim 1
Chromatographic process, it is characterised in that the time of the oscillation extraction is 30min.
6. the application of any one of claim 1 to 5 methods described, it is characterised in that applied to tobacco sample oxalate, amber
The measure of acid group, sulfate radical and/or phosphate radical component.
7. the application of any one of claim 1 to 5 methods described, it is characterised in that added applied to organic acid in tobacco sample
Agent oxalate, amber acid radical, the measure of sulfate radical and/or phosphate radical component.
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Families Citing this family (5)
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| CN108508126A (en) * | 2018-02-12 | 2018-09-07 | 云南中烟工业有限责任公司 | The assay method of non-volatile organic acid in a kind of tobacco gene editor material |
| CN108896697A (en) * | 2018-04-18 | 2018-11-27 | 南京健友生化制药股份有限公司 | Dissociate in a kind of Fondaparinux sodium the detection method of sulfate radical |
| CN108896698B (en) * | 2018-06-05 | 2020-12-04 | 广东中烟工业有限责任公司 | Ion chromatography method for simultaneously determining sorbate acid radicals, phosphate radicals and citrate radicals in reconstituted tobacco and application |
| CN110887930A (en) * | 2019-12-19 | 2020-03-17 | 江苏泰洁智邦检测技术有限公司 | Method for measuring oxalic acid content in workplace |
| 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 |
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