CN105784908B - The chromatography of ions detection method of 6 kinds of anion in cigarette paper - Google Patents
The chromatography of ions detection method of 6 kinds of anion in cigarette paper Download PDFInfo
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- CN105784908B CN105784908B CN201610231248.8A CN201610231248A CN105784908B CN 105784908 B CN105784908 B CN 105784908B CN 201610231248 A CN201610231248 A CN 201610231248A CN 105784908 B CN105784908 B CN 105784908B
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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
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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
- G01N30/04—Preparation or injection of sample to be analysed
- G01N30/06—Preparation
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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
Abstract
The invention discloses a kind of chromatography of ions detection method of 6 kinds of anion in cigarette paper.The present invention is by extractant of ultra-pure water, IonPac AS19 anion-exchange columns are splitter, specific aim optimizes chromatographic condition, and the quantitative analysis of lactate in cigarette paper sample, acetate, formate, chlorion, phosphate radical and citrate is realized using the chromatography of ions.As a result show, the rate of recovery of 6 kinds of anion is between 91.0%~109.5%, and relative standard deviation is between 0.82%~6.26%.The inventive method is accurate, simple, reliable, it is adaptable to the quantitative determination of the especially described 6 kinds of anion of related component in cigarette paper sample.
Description
Technical field
The detection technique field of reconstituted tobacco of the present invention, more particularly, to a kind of ion of 6 kinds of anion in cigarette paper
Chromatographic detection method.
Background technology
Cigarette paper is one of major auxiliary burden of cigarette, directly participates in burning, and its characteristic directly influences the burning of cigarette
Property, fragrance and inhale taste, and be directly connected to the security of cigarette products.Auxiliary agent in cigarette paper is mainly combustionregulator, ash
Divide conditioning agent and a small amount of suction taste conditioning agent, to performance such as main flume, air permeability, the uniformity, burn rate, the bag ash of cigarette paper
Performance etc. plays positive adjustment effect.
Lactate, chlorion and phosphate play a part of adjusting cigarette paper burn rate in cigarette paper, while phosphoric acid
Salt, which is alternatively arranged as ash conditioners, makes ash content solid not loose.Acetate in cigarette paper as combustion adjuvant and ash conditioners,
The burn rate of cigarette paper can be improved；And be bonded together in combustion with pearl filler, grey separation structure is more tied
It is real attractive in appearance without influence of being easily scattered, acetate can be all added in most of cigarette paper as auxiliary agent.Formates can improve cigarette
It is jealous.Citrate is as combustion adjuvant the most frequently used at present, and addition can significantly reduce puff number, tar intake in cigarette paper
Amount, CO growing amounts etc., reduce harm of the smoking to human body and environment.It is some in order to improve cigarette paper in actual production process
The characteristic of aspect, can select to add one or more different auxiliary agents, but cigarette paper is as one of important component of cigarette,
Directly contacted when sucking with mouth, so must be monitored to its security；Meanwhile, the quality and content of auxiliary agent in cigarette paper
Smoking property of cigarette quality can be impacted.Therefore, their contents in cigarette paper and are quickly and accurately analyzed to roll up for monitoring
Quality, the raising tobacco product security of cigarette paper have important effect.
At present, due to the advantages of ion-chromatographic determination is accurate, quick and sensitivity is high, being more applied to cigarette
The measure of anion in paper or tobacco material.But, either the anion of cigarette paper or tobacco material, which is determined, is all mostly
Using AS11-HC anion-exchange columns.AS11-HC has preferable separating effect to most anion, can meet its qualitative fixed
Amount analysis, but the long-term numerous studies of the applicant are summarized and found, the separation of AS11-HC lactates relatively difficult to achieve and acetate.
So, for cigarette paper, the Ion Chromatographic Method for summarizing more science is found, so as to realize cigarette paper sample
In 6 kinds of anion quick and precisely analysis, for monitor cigarette paper quality, improve tobacco product security there is important meaning
Justice.
The content of the invention
The technical problem to be solved in the present invention is the deficiency for being directed to 6 kinds of Anionic recognition technologies in existing cigarette paper, especially
Be in science separation cigarette paper lactate and acetate with the technical deficiency that ensures Detection results, there is provided 6 kinds in a kind of cigarette paper
The chromatography of ions detection method of anion.
The goal of the invention of the present invention is achieved by the following technical programs：
A kind of chromatography of ions detection method of 6 kinds of anion in cigarette paper is provided, cigarette paper sample is obtained after pre-treatment
Sample liquid, sample liquid is through sulfate by ion chromatography, the condition of the sulfate by ion chromatography：
IonPac AS19 anion-exchange columns (4 × 250mm)；KOH leacheates；Flow velocity is 1.5mL/min；Suppress electric current
For 149mA；Column temperature is 23 DEG C；Sample size is 25 μ L；Gradient elution program is shown in Table 1：
The condition of gradient elution of table 1
6 kinds of anion are lactate, acetate, formate, chlorion, phosphate radical and citrate.Described sample
Product pre-treating method is：Cigarette paper sample is added water into (ultra-pure water) after oscillation extraction at room temperature, by extract through 0.45 μm of water
It is to move into chromatogram bottle after membrane filtration, is analyzed by chromatogram condition of work.
Preferably, the amount added water is according to 0.4g cigarette paper samples：The amount of 30mL water is determined.
Preferably, the time of the extraction is 20~50 minutes, more preferably 40 minutes.
Beneficial effects of the present invention：
This area is common to carry out sulfate by ion chromatography anion with sodium hydroxide extraction cigarette paper sample, and the present invention is used
Ultra-pure water carries out oscillation extraction to the acid ion in cigarette paper, and pre-treating method is simple and easy to apply, and reagent safety is convenient, to cigarette
The extraction efficiency of acid ion is notable in paper.The present invention further study show that, ultra-pure water extraction cigarette paper, reached in extraction time
It is maximum to extraction quantity during 40min.Therefore, present invention determine that extraction Best Times be 40min, can extract well target from
Son, it is ensured that single extraction is complete.
The present invention is by carefully studying summary, and preferably IonPac AS19 anion-exchange columns are used as analytical column.With other
Unlike anion quantitative analysis method：Instant invention overcomes custom of this area using " AS11-HC anion analysis post "
Property technology set, creativeness use IonPac AS19 anion-exchange columns for splitter, overcomes AS11-HC anion and divide
Analyse the difficulty of post lactate relatively difficult to achieve and acetate separation.
The further accurate influence for summarizing flow rate of mobile phase and column temperature to Detection results of the invention, is combined a large amount of by research
Experimental summary is obtained, using under the conditions of IonPac AS19 anion-exchange columns, in 1.5mL/min flow velocitys, appearance time compared with
It hurry up, and the requirement of qualitative, quantitative can be met well；Simultaneously best results are separated when column temperature is 23 DEG C；In terms of gradient condition,
During 0~13min, the concentration of KOH leacheates slowly rises to 7mmol/L from 1mmol/L, makes lactate, acetate and first
Acid group is separated, and then the concentration of KOH leacheates is quickly ramped up to 40mmol/L, Cl-、PO4 -It is eluted out with citrate.
By the continuous research and experiment to key factor, the present invention sums up all key factors and interferes or match somebody with somebody
That closes is optimal comprehensive there is provided a kind of new system detecting method, and lactic acid in cigarette paper sample is realized using the chromatography of ions
Root, acetate, formate, chlorion, the quantitative analysis of phosphate radical and citrate, overcome the technology that prior art causes and determine
Gesture, inventive samples pre-treatment is simple, and linear preferable, sample recovery rate is higher, and result of the test of the present invention shows, 6 kinds of anion
The rate of recovery between 91.0%~109.5%, relative standard deviation is between 0.82%~6.26%.Detection method
Accurately, simply, reliably, it is adaptable to the measure of related component in cigarette paper sample, it is especially adapted for use in 6 kinds of the moon in cigarette paper sample
The quantitative analysis of ion, has filled up the blank of prior art.
Brief description of the drawings
The chromatogram of Fig. 1 mixed standard solutions.
Wherein, 1 is lactate, and 2 be acetate, and 3 be formate, and 4 be chlorion, and 5 be phosphate radical, and 6 be citrate.
The chromatogram of Fig. 2 actual samples.
Wherein, 1 is lactate, and 2 be acetate, and 3 be formate, and 4 be chlorion, and 5 be phosphate radical, and 6 be citrate.
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 is obtained, unless stated otherwise, the method and apparatus used in following embodiments are side commonly used in the art
Method and equipment.
Instrument and reagent that the embodiment of the present invention is used：
ICS-5000 types ion chromatograph (DIONEX companies of the U.S.), is equipped with automatic sampler, double pump, automatic leacheate hair
Raw device, electric conductivity detector and the chromatographic work stations of Chromeleon 6.8；Milli-Q ultra-pure waters instrument (Millipore companies of the U.S.)；
CP224S electronic balances (sensibility reciprocal 0.0001g, German Sartorius companies)；(Jiangsu Jin Cheng states win laboratory apparatus to HY-5 oscillators
Factory)；0.45 μm of aqueous phase pin type filter (Town in Shanghai spectrum experiment Science and Technology Co., Ltd.).
Lithium lactate (analyzes pure, Sigma-Aldrich), and sodium acetate (analyzes pure, U.S. Sigma-Aldrich
Company), sodium formate (analyzes pure, Sigma-Aldrich), and (1000mmol/L, country is coloured for chlorion standard liquid
Metal and electronic material Institute of Analysis), phosphate radical standard liquid (1000mmol/L, national non-ferrous metal and electronic material
Institute of Analysis)；Anhydrous citric acid acid (analyzes pure, Sigma-Aldrich)；Ultra-pure water (resistivity >=18.2M
Ω·cm)。
The foundation of the detection method of embodiment 1
1.2 chromatogram conditions of work
IonPac AS19 anion-exchange columns (4 × 250mm)；KOH leacheates；Flow velocity is 1.5mL/min；Suppress electric current
For 149mA；Column temperature is 23 DEG C；Sample size is 25 μ L；Gradient elution program is shown in Table 1.
The condition of gradient elution of table 1
The preparation of 1.3 standard curves
1000 μ g/mL lactate, acetate, formate, chlorion, phosphate radical storing solution and 2000 μ g/ are prepared respectively
ML citrate storing solution, then takes the storing solution of different volumes to be placed in 25mL volumetric flasks, scale is settled to ultra-pure water
Line, shakes up, and is configured to the mixed standard solution of various concentrations.The concentration range of 6 kinds of anion is respectively：Lactate (0~5 μ g/
ML), acetate (0~5 μ g/mL), formate (0~5 μ g/mL), chlorion (0~5 μ g/mL), phosphate radical (0~40 μ g/mL),
Citrate (0~240 μ g/mL).
1.4 sample pre-treatments
0.4g (being accurate to 0.0001g) cigarette paper sample accurately is weighed, is placed in 200mL plastic conicals bottle, it is accurate to add
30mL water, at room temperature oscillation extraction 40min.Extract is moved into chromatogram bottle after 0.45 μm of water system membrane filtration, by color
Spectrum condition of work is analyzed.In recovery of standard addition experiment, 0.4g (being accurate to 0.0001g) cigarette paper sample is accurately weighed,
It is placed in 200mL plastic conicals bottle, then adds 6 kinds of anion standard liquids of various concentrations, add ultra-pure water to 30mL,
Oscillation extraction 40min, chromatography is carried out after crossing 0.45 μm of water system filter membrane at room temperature.
2 results are with discussing
The selection of 2.1 extractants and extraction time
The present invention carries out oscillation extraction using ultra-pure water to the acid ion in cigarette paper, and pre-treating method is simple and easy to apply,
Extraction efficiency to acid ion in cigarette paper is notable.The present invention further study show that, ultra-pure water extraction cigarette paper, extraction
Extraction quantity is maximum when time reaches 40min.Therefore, present invention determine that the Best Times of extraction are 40min, it can extract well
Object ion, it is ensured that single extraction is complete.
0.4000g cigarette paper samples are weighed, at room temperature oscillation extraction, take the extract of extraction different time to carry out respectively
Various experiments under different condition.Research finds that the present invention is using IonPac AS19 anion-exchange columns (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；The gradient elution journey
Under the conditions of sequence, extraction 20,30,40,50min extract can be for carrying out ion chromatography.Further result of the test hair
Existing, 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
AS11-HC anion analysis post has preferable separating effect to most of anion, can meet its qualitative, quantitative
Analysis, but present invention research finds the separation of its lactate and acetate relatively difficult to achieve, for such case, the present invention passes through
Analysis and experiment, it is final to determine to use IonPac AS19 anion-exchange columns, point of lactate and acetate is realized well
From.On this basis, the present invention compare it is different in flow rate under the conditions of separation situation, especially in 1.0mL/min and 1.5mL/
Under two kinds of flow velocitys of min, the separation situation of 6 kinds of anion finds that in 1.5mL/min flow velocitys appearance time is very fast, and meets fixed
The quantitative requirement of property.The optimal column temperature of further analysis and summary is 23 DEG C, then using the work of the chromatograms of Chromeleon 6.8
The Virtual column modules that station is carried have been respectively compared different six kinds of anion of column temperature (23 DEG C, 30 DEG C, 35 DEG C etc.)
Separation situation, demonstrates the separating effect at 23 DEG C preferable.Therefore, the present invention is final determines IonPac AS19 anion exchanges
Post is as analytical column, the chromatographic condition of 1.5mL/min flow velocity and 23 DEG C of column temperature.
The determination of gradient condition：Research is summarized, during 0~13min, the concentration of KOH leacheates from 1mmol/L slowly
7mmol/L is risen to, makes lactate, acetate and formate separation, then the concentration of KOH leacheates is quickly ramped up to 40mmol/L,
Cl-、PO4 -It is eluted out with citrate.Shown in the chromatogram of mixed standard solution and actual sample as Fig. 1 and Fig. 2.
2.3 working curves and test limit
The mixed standard solution prepared is measured by test method, and the peak area and its concentration to each ion enter
Row regression analysis, sets up working curve, and the regression curve of each ion, coefficient correlation are shown in Table 2.
The equation of linear regression and coefficient correlation of 26 kinds of anion of table
| Treat measured ion | Linear equation | Coefficient correlation |
| Lactate | Y=0.1353X-0.0063 | 0.9996 |
| Acetate | Y=0.1693X+0.0099 | 0.9991 |
| Formate | Y=0.1833X-0.0181 | 0.9991 |
| Chlorion | 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 rate of recovery are tested
It is accurate to weigh 3 parts of 0.4000g cigarette paper samples in plastic conical bottle, it is separately added into different amounts of six kinds of standards molten
Liquid, is extracted and is determined by test method, by adding its rate of recovery of the cubage of scalar sum practical measurement (to be shown in Table 3 institutes
Show).As a result show, the rate of recovery of six kinds of anion between 91.0%~109.5%, relative standard deviation 0.82%~
Between 6.26%, illustrate that the inventive method can carry out quantitative analysis.
The rate of recovery of 36 kinds of ions of table
The measure of the actual sample of embodiment 2
Lactate, acetate, formate, chlorine in the cigarette paper sample of 5 kinds of different sizes are determined according to the inventive method
The content of ion, 6 kinds of anion of phosphate radical and citrate, measurement result is shown in Table 4.
As a result show, in the cigarette paper sample of different size, the addition of auxiliary agent differs greatly, such as 1,2, No. 3 samples
In do not detect phosphate radical, and the content of phosphate radical reaches 1.5187mg/g in No. 5 samples；In same cigarette paper sample
In, the addition of each auxiliary agent also has relatively big difference, and such as 2, in No. 3 cigarette paper samples, do not detect phosphate radical, and citrate contains
Amount is respectively 14.7841mg/g, 11.3577mg/g.
The content of 6 kinds of anion in the actual sample of table 4
- represent to be not detected by.
The present invention using the chromatography of ions realize lactate in 5 kinds of cigarette paper samples, acetate, formate, chlorion,
The quantitative analysis of phosphate radical and citrate.From unlike other existing anion quantitative analysis methods：The invention
Ground uses IonPac AS19 anion-exchange columns for splitter, overcomes AS11-HC anion analysis posts lactate relatively difficult to achieve
The difficulty separated with acetate, to the key factor such as the pre-treating method of sample, extraction time, flow velocity and column temperature, elution program
Accurate determination is carried out, the sample pre-treatments of the inventive method are simple, and linear preferable, sample recovery rate is higher, it is adaptable to cigarette
The quantitative analysis of 6 kinds of anion in pattern product.
Claims (2)
1. the chromatography of ions detection method of 6 kinds of anion in a kind of cigarette paper, it is characterised in that 6 kinds of anion are lactic acid
Root, acetate, formate, chlorion, phosphate radical and citrate；Cigarette paper sample obtains sample after extracting pre-treatment through ultra-pure water
Product liquid, sample liquid is through sulfate by ion chromatography, the condition of the sulfate by ion chromatography：
4 × 250mm IonPac AS19 anion-exchange columns；KOH leacheates；Flow velocity is 1.5mL/min；Suppressing electric current is
149mA；Column temperature is 23 DEG C；Sample size is 25 μ L；Gradient elution program is：
The sample-pretreating method is：Add ultra-pure water after oscillation extraction at room temperature in cigarette paper sample, extract is passed through
Move into and analyzed in chromatogram bottle after 0.45 μm of water system membrane filtration；The time of the extraction is 40 minutes.
2. according to claim 1 in cigarette paper 6 kinds of anion chromatography of ions detection method, it is characterised in that it is plus ultrapure
The amount of water is according to 0.4g cigarette paper samples：The amount of 30mL ultra-pure waters is determined.
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| CN106442798B (en) * | 2016-11-04 | 2018-12-14 | 长沙理工大学 | A kind of accurate measuring method of humic-acid kind organic matter high-temperature decomposition product |
| 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 |
| 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 |
| CN113092650B (en) * | 2021-04-16 | 2022-04-19 | 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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| CN102253153B (en) * | 2011-04-11 | 2014-06-04 | 浙江大学 | Method for optimizing gradient elution condition of ion chromatographic determination of anion in tobacco leaf by response surface methodology |
| DE102011056290A1 (en) * | 2011-12-12 | 2013-06-13 | Thyssenkrupp Uhde Gmbh | MUSHROOMS WITH GENETIC MODIFICATION CONCERNING A CARBONIC ACID TRANSPORTER |
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