CN105784908A - Ion chromatography detection method for six negative ions in cigarette paper - Google Patents
Ion chromatography detection method for six negative ions in cigarette paper Download PDFInfo
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- 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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- 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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- 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
- G01N30/88—Integrated analysis systems specially adapted therefor, not covered by a single one of the groups G01N30/04 - G01N30/86
- G01N2030/8809—Integrated analysis systems specially adapted therefor, not covered by a single one of the groups G01N30/04 - G01N30/86 analysis specially adapted for the sample
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Abstract
The invention discloses an ion chromatography detection method for six negative ions in cigarette paper.Ultrapure water is adopted as an extracting agent, IonPac AS19 negative ion exchange columns are separation columns, chromatographic conditions are optimized in a targeted mode, and the ion chromatography is adopted for achieving quantitative analysis of lactate, acetate, formate, chloridion, phosphate radicals and citrate in cigarette paper samples.A result shows that the recycling rates of the six negative ions range from 91.0% to 109.5%, and the relative standard deviation ranges from 0.82% to 6.26%.The method is accurate, simple, reliable and applicable to quantitative determination of relative components, particularly six negation ions in the cigarette paper samples.
Description
Technical field
The detection technique field of reconstituted tobacco of the present invention, more particularly, to the chromatography of ions detection method of 6 kinds of aniones in a kind of cigarette paper.
Background technology
Cigarette paper is one of major auxiliary burden of cigarette, directly participates in burning, and its characteristic directly influences the flammability of Medicated cigarette, fragrance and suction taste, and is directly connected to the safety of cigarette products.Auxiliary agent in cigarette paper is mainly combustionregulator, ash conditioners and a small amount of suction taste regulator, and the performance such as main flume, air permeability of cigarette paper, the uniformity, burn rate, bag ash performance etc. are played positive adjustment effect.
Lactate, chloride ion and phosphate play the effect regulating cigarette paper burn rate in cigarette paper, and simultaneously phosphate is alternatively arranged as ash conditioners and makes ash solid not loose.Acetate as combustion adjuvant and ash conditioners, can improve the burn rate of cigarette paper in cigarette paper；And be bonded together with pearl filler in combustion, make ash separation structure more solid and not easily be scattered impact attractive in appearance, major part cigarette paper in all can add acetate as auxiliary agent.Formates can improve the jealous of Medicated cigarette.Citrate, as combustion adjuvant the most frequently used at present, is added in cigarette paper and can significantly reduce puff number, tar intake, CO growing amount etc., reduces the smoking harm to human body and environment.In actual production process, in order to improve the characteristic of some aspect of cigarette paper, can select to add one or more different auxiliary agents, but cigarette paper is as one of the important component part of Medicated cigarette, directly contacts with mouth when sucking, so must its safety be monitored；Meanwhile, in cigarette paper, smoking property of cigarette quality can be impacted by the quality of auxiliary agent and content.Therefore, analyze they content in cigarette paper and quickly and accurately, for monitoring the quality of cigarette paper, improving tobacco product safety, there is important effect.
At present, due to ion-chromatographic determination accurately, quickly and sensitivity advantages of higher, more it is applied in cigarette paper or tobacco material the mensuration of anion.But, it is that the anion mensuration of cigarette paper or tobacco material is all adopt AS11-HC anion-exchange column mostly.Most aniones are all had good separating effect by AS11-HC, can meet its qualitative and quantitative analysis, but the applicant's a large amount of research summaries for a long time find, the more difficult separation realizing lactate and acetate of AS11-HC.
So, for cigarette paper, find the Ion Chromatographic Method of science more of summing up, thus realizing the quick and precisely analysis of 6 kinds of aniones in cigarette paper sample, for monitoring the quality of cigarette paper, to improve tobacco product safety significant.
Summary of the invention
The technical problem to be solved in the present invention is for the deficiency of 6 kinds of Anionic recognition technology in existing cigarette paper, especially in science separation cigarette paper lactate and acetate to ensure the technical deficiency of Detection results, it is provided that the chromatography of ions detection method of 6 kinds of aniones in a kind of cigarette paper.
The goal of the invention of the present invention is achieved by the following technical programs:
Thering is provided the chromatography of ions detection method of 6 kinds of aniones in a kind of cigarette paper, cigarette paper sample obtains sample liquid after pre-treatment, and sample liquid is through sulfate by ion chromatography, and the condition of described sulfate by ion chromatography is:
IonPacAS19 anion-exchange column (4 × 250mm)；KOH leacheate；Flow velocity is 1.5mL/min；Suppression electric current is 149mA；Column temperature is 23 DEG C；Sample size is 25 μ L；Gradient elution program is shown in Table 1:
Table 1 condition of gradient elution
Described 6 kinds of aniones are lactate, acetate, formate, chloride ion, phosphate radical and citrate.Described sample-pretreating method is: after cigarette paper sample is added water (ultra-pure water) under room temperature oscillation extraction, extract is moved in chromatogram bottle after 0.45 μm of water system membrane filtration, is analyzed by chromatograph working condition.
Preferably, the amount added water is according to 0.4g cigarette paper sample: the amount of 30mL water is determined.
Preferably, the time of described extraction is 20～50 minutes, more preferably 40 minutes.
Beneficial effects of the present invention:
This area is common carries out sulfate by ion chromatography anion with sodium hydroxide extraction cigarette paper sample, the present invention adopts ultra-pure water that the acid ion in cigarette paper is carried out oscillation extraction, pre-treating method is simple, and reagent safety is convenient, and the extraction efficiency of acid ion in cigarette paper is notable.The present invention further study show that, ultra-pure water extracts cigarette paper, and when extraction time reaches 40min, extraction quantity is maximum.Therefore, present invention determine that the Best Times of extraction is 40min, it is possible to extract object ion well, it is ensured that single extraction is complete.
The present invention is through carefully studying summary, it is preferable that IonPacAS19 anion-exchange column is as analytical column.With other anion quantitative analysis methods the difference is that: instant invention overcomes this area adopt " AS11-HC anion analysis post " habitually technology set, creative to adopt IonPacAS19 anion-exchange column be detached dowel, overcomes that AS11-HC anion analysis post is more difficult realizes the difficulty that lactate separates with acetate.
The present invention accurately sums up flow rate of mobile phase and the column temperature impact on Detection results further, obtain in conjunction with great many of experiments summary through research, under utilizing IonPacAS19 anion exchange column condition, when 1.5mL/min flow velocity, appearance time is very fast, and can meet the requirement of qualitative, quantitative well；Separate best results when column temperature is 23 DEG C simultaneously；Gradient condition aspect, during 0～13min, the concentration of KOH leacheate rises to 7mmol/L lentamente from 1mmol/L, makes lactate, acetate separate with formate, and then the concentration of KOH leacheate is quickly ramped up to 40mmol/L, Cl-、PO4 -It is eluted out with citrate.
By constantly studying and test key factor, the present invention sum up all key factors interfere or coordinate best comprehensive, provide a kind of new system detecting method, the chromatography of ions is adopted to achieve lactate in cigarette paper sample, acetate, formate, chloride ion, the quantitative analysis of phosphate radical and citrate, overcome the technology set that prior art causes, inventive samples pre-treatment is simple, linear desirable, sample recovery rate is higher, result of the test of the present invention shows, the response rate of 6 kinds of aniones is between 91.0%～109.5%, relative standard deviation is between 0.82%～6.26%.Detection method accurately, simple, reliable, it is adaptable to the mensuration of related component in cigarette paper sample, be especially adapted for use in cigarette paper sample the quantitative analysis of 6 kinds of aniones, filled up the blank of prior art.
Accompanying drawing explanation
The chromatogram of Fig. 1 mixed standard solution.
Wherein, 1 is lactate, and 2 is acetate, and 3 is formate, and 4 is chloride ion, and 5 is phosphate radical, and 6 is citrate.
The chromatogram of Fig. 2 actual sample.
Wherein, 1 is lactate, and 2 is acetate, and 3 is formate, and 4 is chloride ion, and 5 is phosphate radical, and 6 is citrate.
Detailed description of the invention
The present invention is further illustrated below in conjunction with the drawings and specific embodiments.Following embodiment being merely cited for property explanation, it is impossible to be interpreted as limitation of the present invention.Unless stated otherwise, the reagent used in following embodiment is reagent that is conventional commercial or that be either commercially available, and unless stated otherwise, the method and apparatus used in following embodiment is method and apparatus commonly used in the art.
The instrument of embodiment of the present invention employing and reagent:
ICS-5000 type ion chromatograph (DIONEX company of the U.S.), is equipped with automatic sampler, double pump, automatic leacheate generator, electric conductivity detector and Chromeleon6.8 chromatographic work station；Milli-Q ultra-pure water instrument (Millipore company of the U.S.)；CP224S electronic balance (sensibility reciprocal 0.0001g, Sartorius company of Germany)；HY-5 agitator (Jiangsu Jin Cheng Guo Sheng experimental apparatus factory)；0.45 μm of aqueous phase pin type filter (Town in Shanghai spectrum tests Science and Technology Co., Ltd.).
EINECS 212-761-8 (analytical pure, Sigma-Aldrich), sodium acetate (analytical pure, Sigma-Aldrich), sodium formate (analytical pure, Sigma-Aldrich), chloride ion standard solution (1000mmol/L, country's non-ferrous metal and electronic material Institute of Analysis), phosphate radical standard solution (1000mmol/L, country's non-ferrous metal and electronic material Institute of Analysis)；Anhydrous citric acid acid (analytical pure, Sigma-Aldrich)；Ultra-pure water (resistivity >=18.2M Ω cm).
The foundation of embodiment 1 detection method
1.2 chromatograph working condition
IonPacAS19 anion-exchange column (4 × 250mm)；KOH leacheate；Flow velocity is 1.5mL/min；Suppression electric current is 149mA；Column temperature is 23 DEG C；Sample size is 25 μ L；Gradient elution program is in Table 1.
Table 1 condition of gradient elution
The preparation of 1.3 standard curves
Prepare the citrate storing solution of the lactate of 1000 μ g/mL, acetate, formate, chloride ion, phosphate radical storing solution and 2000 μ g/mL respectively, then the storing solution taking different volumes is placed in 25mL volumetric flask, it is settled to graduation mark with ultra-pure water, shake up, be configured to the mixed standard solution of variable concentrations.The concentration range of 6 kinds of aniones is respectively as follows: lactate (0～5 μ g/mL), acetate (0～5 μ g/mL), formate (0～5 μ g/mL), chloride ion (0～5 μ g/mL), phosphate radical (0～40 μ g/mL), citrate (0～240 μ g/mL).
1.4 sample pre-treatments
Accurately weigh 0.4g (being accurate to 0.0001g) cigarette paper sample, be placed in 200mL plastic conical bottle, accurately add 30mL water, oscillation extraction 40min under room temperature.Extract is moved in chromatogram bottle after 0.45 μm of water system membrane filtration, is analyzed by chromatograph working condition.In recovery of standard addition is tested, accurately weigh 0.4g (being accurate to 0.0001g) cigarette paper sample, it is placed in 200mL plastic conical bottle, it is subsequently adding 6 kinds of anion standard solution of variable concentrations, add ultra-pure water to 30mL, oscillation extraction 40min under room temperature, carries out chromatography after crossing 0.45 μm of water system filter membrane.
2 results and discussion
The selection of 2.1 extractants and extraction time
The present invention adopts ultra-pure water that the acid ion in cigarette paper is carried out oscillation extraction, and pre-treating method is simple, and the extraction efficiency of acid ion in cigarette paper is notable.The present invention further study show that, ultra-pure water extracts cigarette paper, and when extraction time reaches 40min, extraction quantity is maximum.Therefore, present invention determine that the Best Times of extraction is 40min, it is possible to extract object ion well, it is ensured that single extraction is complete.
Weigh 0.4000g cigarette paper sample, oscillation extraction under room temperature, take respectively and extract the various tests that the extract of different time carries out under different condition.Research finds, the present invention adopts IonPacAS19 anion-exchange column (4 × 250mm)；KOH leacheate；Flow velocity is 1.5mL/min；Suppression electric current is 149mA；Column temperature is 23 DEG C；Sample size is 25 μ L；When described gradient elution program, extract 20,30,40, the extract of 50min can be used to carry out ion chromatography.Further result of the test finds, when extraction time reaches 40min, extraction quantity is maximum.Therefore, present invention determine that extraction time is 40min.
The selection of 2.2 chromatographic conditions
Most of aniones are all had good separating effect by AS11-HC anion analysis post, its qualitative and quantitative analysis can be met, but the present invention studies its more difficult separation realizing lactate and acetate of discovery, for this situation, the present invention by analysis and tests, finally determine employing IonPacAS19 anion-exchange column, achieve the separation of lactate and acetate well.On this basis, the present invention compares separation case when different in flow rate, particularly under two kinds of flow velocitys of 1.0mL/min and 1.5mL/min, the separation case of 6 kinds of aniones, finding when 1.5mL/min flow velocity, appearance time is very fast, and meets the requirement of qualitative, quantitative.The best column temperature of further analysis and summary is 23 DEG C, then adopt the Virtualcolumn module that carries of Chromeleon6.8 chromatographic work station to be respectively compared the separation case of six kinds of aniones of different column temperature (23 DEG C, 30 DEG C, 35 DEG C etc.), demonstrate the separating effect when 23 DEG C better.Therefore, the present invention finally determines that IonPacAS19 anion-exchange column is as analytical column, the chromatographic condition of the column temperature of the flow velocity of 1.5mL/min and 23 DEG C.
The determination of gradient condition: research summary, during 0～13min, the concentration of KOH leacheate rises to 7mmol/L lentamente from 1mmol/L, makes lactate, acetate separate with formate, and then the concentration of KOH leacheate is quickly ramped up to 40mmol/L, Cl-、PO4 -It is eluted out with citrate.The chromatogram of mixed standard solution and actual sample is shown in shown in Fig. 1 and Fig. 2.
2.3 working curves and detection limit
Being measured by test method by the mixed standard solution prepared, and the peak area and its concentration to each ion carries out regression analysis, sets up working curve, the regression curve of each ion, correlation coefficient are shown in Table 2.
The equation of linear regression of 26 kinds of aniones of table and correlation coefficient
| Treat measured ion | Linear equation | Correlation coefficient |
| Lactate | Y=0.1353X-0.0063 | 0.9996 |
| Acetate | Y=0.1693X+0.0099 | 0.9991 |
| Formate | Y=0.1833X-0.0181 | 0.9991 |
| Chloride ion | Y=0.4086X-0.0204 | 0.9998 |
| Phosphate radical | Y=0.1202X-0.0745 | 0.9996 |
| Citrate | Y=0.0758X+0.3485 | 0.9994 |
2.4 response rate experiments
Accurately weigh 3 parts of 0.4000g cigarette paper samples in plastic conical bottle, be separately added into different amounts of six kinds of standard solution, undertaken extracting and measuring by test method, by adding its response rate of the cubage (being shown in Table 3) of scalar sum practical measurement.It is shown that the response rate of six kinds of aniones is between 91.0%～109.5%, relative standard deviation, between 0.82%～6.26%, illustrates that the inventive method can carry out quantitative analysis.
The response rate of 36 kinds of ions of table
The mensuration of embodiment 2 actual sample
Determine the content of lactate in the cigarette paper sample of 5 kinds of different sizes, acetate, formate, chloride ion, phosphate radical and 6 kinds of aniones of citrate according to the inventive method, measurement result is shown in Table 4.
It is shown that in the cigarette paper sample of different size, the addition of auxiliary agent differs greatly, in 1,2, No. 3 samples, all do not detect phosphate radical, and in No. 5 samples, the content of phosphate radical reaches 1.5187mg/g；In same cigarette paper sample, the addition of each auxiliary agent also has relatively big difference, in 2, No. 3 cigarette paper samples, does not detect phosphate radical, and the content of citrate respectively 14.7841mg/g, 11.3577mg/g.
The content of 6 kinds of aniones in table 4 actual sample
-expression is not detected by.
The present invention adopts the chromatography of ions to achieve the quantitative analysis of lactate, acetate, formate, chloride ion, phosphate radical and citrate in 5 kinds of cigarette paper samples.With other anion quantitative analysis methods existing the difference is that: the present invention creatively adopts IonPacAS19 anion-exchange column to be detached dowel, overcome that AS11-HC anion analysis post is more difficult realizes the difficulty that lactate separates with acetate, carry out accurately determining to the pre-treating method of sample, extraction time, flow velocity and the key factor such as column temperature, elution program, the sample pre-treatments of the inventive method is simple, linear desirable, sample recovery rate is higher, it is adaptable to the quantitative analysis of 6 kinds of aniones in cigarette paper sample.
Claims (4)
1. the chromatography of ions detection method of 6 kinds of aniones in a cigarette paper, it is characterised in that described 6 kinds of aniones are lactate, acetate, formate, chloride ion, phosphate radical and citrate；Cigarette paper sample extracts through ultra-pure water and obtains sample liquid after pre-treatment, and sample liquid is through sulfate by ion chromatography, and the condition of described sulfate by ion chromatography is:
IonPacAS19 anion-exchange column (4 × 250mm)；KOH leacheate；Flow velocity is 1.5mL/min；Suppression electric current is 149mA；Column temperature is 23 DEG C；Sample size is 25 μ L；Gradient elution program is:
Time (min) KOH solution concentration (mmol/L)
01；
137；
1540；
2440；
24.011；
291。
2. the chromatography of ions detection method of 6 kinds of aniones in cigarette paper according to claim 1, it is characterized in that, described sample-pretreating method is: cigarette paper sample adds after ultra-pure water oscillation extraction under room temperature, is moved in chromatogram bottle by extract and be analyzed after 0.45 μm of water system membrane filtration.
3. the chromatography of ions detection method of 6 kinds of aniones in cigarette paper according to claim 2, it is characterised in that the amount added water is according to 0.4g cigarette paper sample: the amount of 30mL water is determined.
4. the chromatography of ions detection method of 6 kinds of aniones in cigarette paper according to claim 1 or claim 2, it is characterised in that the time of described extraction is 40 minutes.
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| CN106442798A (en) * | 2016-11-04 | 2017-02-22 | 长沙理工大学 | Accurate determination method for high-temperature decomposition products of humic acid organic matters |
| CN108896699A (en) * | 2018-07-06 | 2018-11-27 | 北京城市排水集团有限责任公司 | The detection method of sodium acetate in a kind of sewage |
| CN108896698A (en) * | 2018-06-05 | 2018-11-27 | 广东中烟工业有限责任公司 | Ion chromatographic method and application a kind of while that measure sorb acid group in reconstituted tobacco, phosphate radical and citrate |
| 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 |
| CN113092650A (en) * | 2021-04-16 | 2021-07-09 | 云南中烟工业有限责任公司 | Detection method of raspberry glycoside in cigarette paper |
| CN113109496A (en) * | 2021-04-20 | 2021-07-13 | 陕西中烟工业有限责任公司 | Ion chromatography determination method for 8 anions and acid radical ions in cigarette paper |
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| CN106442798A (en) * | 2016-11-04 | 2017-02-22 | 长沙理工大学 | Accurate determination method for high-temperature decomposition products of humic acid organic matters |
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| CN108896698A (en) * | 2018-06-05 | 2018-11-27 | 广东中烟工业有限责任公司 | Ion chromatographic method and application a kind of while that measure sorb acid group in reconstituted tobacco, phosphate radical and citrate |
| CN108896699A (en) * | 2018-07-06 | 2018-11-27 | 北京城市排水集团有限责任公司 | The detection method of sodium acetate in a kind of sewage |
| 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 |
| CN113092650A (en) * | 2021-04-16 | 2021-07-09 | 云南中烟工业有限责任公司 | Detection method of raspberry glycoside in cigarette paper |
| CN113109496A (en) * | 2021-04-20 | 2021-07-13 | 陕西中烟工业有限责任公司 | Ion chromatography determination method for 8 anions and acid radical ions in cigarette paper |
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