CN106645503B - Li in packaging bag containing cigarette+、Na+、NH4+、K+、Mg2+、Ca2+The content assaying method of ion - Google Patents
Li in packaging bag containing cigarette+、Na+、NH4+、K+、Mg2+、Ca2+The content assaying method of ion Download PDFInfo
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- CN106645503B CN106645503B CN201710110796.XA CN201710110796A CN106645503B CN 106645503 B CN106645503 B CN 106645503B CN 201710110796 A CN201710110796 A CN 201710110796A CN 106645503 B CN106645503 B CN 106645503B
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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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- 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
- G01N30/04—Preparation or injection of sample to be analysed
- G01N30/06—Preparation
- G01N2030/062—Preparation extracting sample from raw material
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Abstract
The invention discloses Li in a kind of packaging bag containing cigarette+、Na+、NH4 +、K+、Mg2+、Ca2+The content assaying method of ion.This method comprises the following steps: (1) preparation of testing sample solution;(2) it is detected using ion chromatography;The preparation of testing sample solution described in step (1) method particularly includes: will contain after cigarette packaging bag extracts with extractant, extract liquor filter membrane is to get the testing sample solution;The extractant includes stabilizer, alcohol, acid and water.This method uses IC method for the first time while measuring the content of a variety of cations in packaging bag containing cigarette, and this method has filled up prior art blank;And this method has the characteristics that sample analysis flux big, accuracy and reproducible.
Description
Technical field
The present invention relates to composition measurement technical fields in smoke-free tobacco product adjuvant materials, and in particular to a kind of packet containing cigarette
Li in pack+、Na+、NH4 +、K+、Mg2+、Ca2+The content assaying method of ion.
Background technique
Without burning or not when smoke-free tobacco product (Smokeless tobacco products, STPs) refers to use
The tobacco product for generating flue gas, can be divided into mouth type (Oral STPs) and nose type (Nasal STPs) two according to usage mode
Big type.Mouthful include chewing tobacco (Chewing tobacco), containing the multiple types such as cigarette, molten cigarette with type STPs, wherein containing cigarette be its most
Main product form has American Moist Snuff type to contain two kinds of cigarette containing cigarette, Sweden's Snus type, and the usage mode of the two is all
It is put between gum and lip, it is entirely different with traditional snuff (Nasal tobacco).Each domestic mouth containing type smokeless tobacco in Northern Europe
Product belongs to Swedish Snus type, and sample pH value is within the scope of neutral meta-alkalescence;The U.S. produces buccal smokeless tobacco product
Existing American Moist Snuff, and have Swedish Snus, therefore, pH wider range of sample.
Buccal smokeless tobacco product is divided into bulk and packed two major classes from the packaging, referred to as in bulk containing cigarette and packed to contain
Cigarette.It is in bulk to contain cigarette containing cigarette (Loose Tobacco) for tradition, it is divided into crin (Long Cut) and filament (Fine Cut), uses
When, take it is a handful of be placed between lip and gum, gently suck make tobacco or fragrance component through saliva between teeth space enter oral cavity, produce
Raw organoleptic effect.The behavior that such product spues after is most unseemly, and has dregs residual.The packed of modern production contains cigarette
(Pouch Tobacco) is charged material into penetrability pouch, is not only easy to use consumption, but also will not pollute oral cavity.In recent years, respectively
Big tobacco enterprise is developed one after another and the bagged product for the famous brand name that releases one after another, such as R. J. Reynolds Tobacco release " camel " card series bag
Dress is packed containing cigarette etc. containing cigarette, luxuriant and rich with fragrance not tobacco release " Marlboro " card series.
In recent years, global tobacco control dynamics constantly enhances, and smoke-free tobacco product has been increasingly becoming the important tobacco of one kind and has disappeared
Fei Pin, and represent the important trend of international Field of Tobacco.But there is presently no to smoke-free tobacco product auxiliary material
Ingredient and its containing quantifier elimination report.
It is packed to contain penetrability pouch used in cigarette (Pouch Tobacco), it, may directly with the oral contact of consumer
Mouthfeel containing cigarette, taste can be impacted, ingredient may also can affect to consumer.Especially Li+、Na+、NH4 +、K+、Mg2+、Ca2+It is affected Deng cation to consumer, therefore, it is necessary to monitor above-mentioned in packaging bag containing cigarette
Ingredient.
Summary of the invention
The purpose of the present invention is to provide Li in a kind of packaging bag containing cigarette+、Na+、NH4 +、K+、 Mg2+、Ca2+The content of ion
Measuring method, to solve the problems, such as that the prior art lacks to cation detections a variety of in packaging bag containing cigarette.
To achieve the above object, the method for the present invention is achieved by the following technical programs:
Li in one kind packaging bag containing cigarette+、Na+、NH4 +、K+、Mg2+、Ca2+The content assaying method of ion includes following step
It is rapid:
(1) preparation of testing sample solution;
(2) it is detected using ion chromatography;
The preparation of testing sample solution described in step (1) method particularly includes: cigarette packaging bag will be contained and extracted with extractant
Afterwards, extract liquor filter membrane is to get the testing sample solution;The extractant includes stabilizer, alcohol, acid and water.
When detecting the specific ingredient in different samples using ion chromatography, several ingredients, pre-treatment can be measured simultaneously
Journey is particularly significant.How to be extracted from the sample of complicated component need the ingredient that measures be can realize while detect it is a variety of at
The key divided.And in the present invention, the ingredient in packaging bag containing cigarette is sufficiently complex, how and meanwhile successfully extract packaging bag containing cigarette
In a variety of cation (such as Li+、Na+、NH4 +、K+、Mg2+、Ca2+Ion is the problem that must be broken through first when detection, inventor
Grope through largely testing, has extracted 6 kinds of ions in packaging bag containing cigarette: Li simultaneously by the above method+、Na+、NH4 +、K+、Mg2+、Ca2+Ion, and then realize and utilize ion chromatography for the first time while measuring Li in packaging bag containing cigarette+、Na+、NH4 +、K+、Mg2 +、Ca2+The content of ion has filled up prior art blank.
Preferably, in extractant:
The stabilizer selects liquid stabilisers or Pickering agent;
When stabilizer selects liquid stabilisers, liquid stabilisers: alcohol: acid: water=0-1000 mL:0-1000mL:0-
100mL:1000mL;
When stabilizer selects Pickering agent, Pickering agent: alcohol: acid: water=0-5g:0-1000mL:0-100mL:
1000mL;
The liquid stabilisers are selected from alcohols, ketone or aldehydes;The alcohols is selected from methanol, ethyl alcohol and/or the third three
Alcohol, the ketone are selected from acetone and/or butanone, and the aldehydes is selected from formaldehyde, acetaldehyde and/or propionic aldehyde;
The Pickering agent is selected from paraformaldehyde;
The alcohol is selected from methanol, ethyl alcohol and/or glycerine;
The acid is selected from nitric acid, hydrochloric acid, sulfuric acid and/or perchloric acid.
Preferably, nitric acid described in extractant refers to that mass fraction is the concentrated nitric acid of 60-65%;The hydrochloric acid refers to
Mass fraction is the concentrated hydrochloric acid of 30-38%;The sulfuric acid refers to the concentrated sulfuric acid that mass fraction is about 90-98%;The height
Chloric acid refers to the perchloric acid that mass fraction is about 65-75%.
Above-mentioned extract liquor is that inventor screens through many experiments, in above-mentioned extract liquor and cooperation institute of the present invention
The extraction conditions stated can guarantee Li in packaging bag containing cigarette+、Na+、NH4 +、K+、 Mg2+、Ca2+Ion extractuin is complete, while can also be with
Play effect cationic in stable sample, it is ensured that assay result is stablized in sample in r for 24 hours, extends effectively
The holding time of sample solution greatly increases daily sample amount detection.
Preferably, the preparation of testing sample solution described in step (1) method particularly includes:
Cigarette packaging bag will be contained to be placed in collection vessel, addition extractant, after ultrasound or oscillation extraction, extract liquor filter membrane,
Up to the testing sample solution;The collection vessel selects the container made of acid-fast alkali-proof plastics.
It is further preferred that the acid-fast alkali-proof plastics are polyethylene or polytetrafluoroethylene (PTFE).
Above-mentioned acid-fast alkali-proof plastics are selected to can avoid introducing Na due to the factor of container material quality during the experiment+Ion
Equal interfering substances, influence the accuracy of detection, lead to the Na in packaging bag containing cigarette+The content detection of ion is worth higher system and misses
Difference.
Preferably, the amount ratio of the packaging bag containing cigarette and extractant is 0.01-5g:5-100 mL, and extraction time is
10-60min places 0-10min after extraction.
Preferably, the filtering uses aperture to carry out for 0.22 or 0.45 μm of filter membrane, filter membrane material selection polyether sulfone
(PES) filter membrane, hydrophilic Kynoar (PVDF) filter membrane or nylon66 fiber filter membrane.
Preferably, the specific testing conditions of ion chromatography described in step (2) are as follows: chromatographic column selects cation analysis
Column;Flow velocity is 0.5-2mL/min;Sample volume is 25-100 μ L;Column temperature is 20-39 DEG C;Detection cell temperature is 20-39 DEG C;Inhibit
Device electric current is 2-300mA;Gradient is 0.001-0.035mol/L MAS isocratic elution or gradient elution program.
It is further preferred that the specific testing conditions of ion chromatography described in step (2) are as follows: chromatographic column selection CS12A,
CS16 or CS19 cation analysis column;Flow velocity is 0.4-1.5 mL/min;Column temperature is 30-35 DEG C;Detection cell temperature is 30-35
℃;Suppressor electric current is 20-120 mA;Detector selects electric conductivity detector;Suppressor selects CSRS-II;Guard column is selected
CG12A, CG16 or CG19 cation guard column;Instrument model is ICS-5000 or ICS-3000 plasma chromatography instrument.
It is further preferred that gradient elution program described in step (2) are as follows: when 0min, the concentration of MAS is
18.0mmol/L;When 14.0min, the concentration of MAS is 18.0mmol/L;When 14.1 min, the concentration of MAS is 24.0mmol/L;
When 18.0min, the concentration of MAS is 24.0 mmol/L;When 18.1min, the concentration of MAS is 18.0mmol/L;20.0min when,
The concentration of MAS is 18.0mmol/L.
MAS of the present invention refers to Loprazolam aqueous solution.
When detecting the specific ingredient in different samples using ion chromatography, the selection of testing conditions is also extremely important, detection
Condition selection is incorrect or selection testing conditions have differences, and can all cause ingredient to be measured to be surveyed ineffective;Such as quasi-molecular ions point
It does not open, the problems such as sensitivity is not high.Inventor has found after a lot of trial and error, under above-mentioned specific testing conditions simultaneously
Detect cation Li in 6 in packaging bag containing cigarette+、Na+、NH4 +、K+、Mg2+、Ca2+The content of ion has optimal quasi-molecular ions
Separating degree, sensitivity and selectivity.
Preferably, the content assaying method, further includes quantitative analysis step, and the quantitative analysis uses external standard method
Or internal standard method.
Most preferably, the quantitative analysis uses external standard method, and the specific method is as follows:
A series of standard working solution for preparing reference substances containing various concentration object establishes standard using IC method
Working curve, the quantitative detection for sample;Cations in sample are calculated by formula (1);
Ci=CI is surveyed*V/n.................................................(1)
In formula, CiFor the quality of cationic substance i in every gram of packed sample of packaging bag containing cigarette to be measured, unit mg/g, knot
Fruit is accurate to 0.01mg/g;
CI is surveyedThe content of resulting cationic substance i, unit mg/g are measured for IC;
V is extractant volume, unit mL;
N is the weight for carrying out the packed sample of packaging bag containing cigarette of this analysis, unit g;
Take the arithmetic mean of instantaneous value of two parallel samples as test result to get into the packed sample of packaging bag containing cigarette to be measured
Li+、Na+、NH4 +、K+、Mg2+、Ca2+The content of ion.
The method of the present invention has the advantages that (1) content assaying method of the present invention uses IC method for the first time while surveying
Surely a variety of cation (predominantly Li in packaging bag containing cigarette+、Na+、NH4 +、K+、 Mg2+、Ca2+) content, this method filled up existing
There is technological gap;(2) sample pretreatment process of the present invention is simple, and detection efficiency is high;(3) pre-treating method of the present invention can be protected
Demonstrate,prove Li in packaging bag containing cigarette+、Na+、NH4 +、K+、Mg2+、Ca2+Ion extractuin is complete, at the same can also play stable sample middle-jiao yang, function of the spleen and stomach from
The effect of son, it is ensured that assay result is stablized in sample in r for 24 hours, extends the holding time of effective sample solution,
Greatly increase daily sample amount detection;(4) this method has sample analysis flux big, and accuracy, reproducible
Feature.
Detailed description of the invention
Fig. 1 is Li in packaging bag containing cigarette+、Na+、NH4 +、K+、Mg2+、Ca2+The content determination chromatogram of ion standard solution.
Fig. 2 is Li in packaging bag containing cigarette+、Na+、NH4 +、K+、Mg2+、Ca2+Determination of ion content chromatogram.
Specific embodiment
The following examples are used to illustrate the present invention, but are not intended to limit the scope of the present invention..
Li in 1 packaging bag containing cigarette of embodiment+、Na+、NH4 +、K+、Mg2+、Ca2+The assay of ion standard solution
(1) standard solution sample preparation condition:
Using polytetrafluoroethylene (PTFE) (PETT) volumetric flask, Li is prepared with extract liquor+、Na+、NH4 +、 K+、Mg2+、Ca2+Ion is dense
Degree is the standard solution of 2 μ g/mL.
Extract liquor are as follows: methanol: ethyl alcohol: hydrochloric acid (selects the concentrated hydrochloric acid that mass fraction is about 35.5%): water, by 500mL:
500mL:2.6mL:1000mL mixing.After shaken at room temperature 10min, extract liquor passes through 0.22 μm of hydrophilic Kynoar (PVDF)
Filter membrane is collected filtered extract liquor and is placed in ion chromatography bottle as sample, to be detected.
(2) sample ions chromatography IC is detected:
Chromatographic column: CS19 analytical column is equipped with CG19 guard column;Flow velocity: 1.0mL/min;Sample volume: 100 μ L;Column temperature: 35
℃;Detection cell temperature: 39 DEG C;Detector: electric conductivity detector;Suppressor: CSRS-II;Suppressor electric current: 108mA;Elute journey
Sequence: (MSA) 0.020mol/L MAS isocratic elution.
Li in packaging bag containing cigarette+、Na+、NH4 +、K+、Mg2+、Ca2+The chromatogram of the assay of ion standard solution is shown in figure
1。
Li in 2 sample of packaging bag containing cigarette of embodiment+、Na+、NH4 +、K+、Mg2+、Ca2+Determination of ion content
(1) preparation of testing sample solution;
(2) it is detected using ion chromatography;
(3) quantitative analysis;
The preparation of testing sample solution in step (1) method particularly includes: accurately weigh the packed sample of packaging bag containing cigarette
0.2g is put into 100mL tool plug polytetrafluoroethylene (PTFE) triangular flask, 50mL extractant is added, and shaken at room temperature extracts 40min, places
After 5min, extract liquor collects filtered extract liquor as sample and is placed in ion by 0.45 μm of polyether sulfone (PES) membrane filtration
In chromatogram bottle, testing sample solution is obtained;Wherein, extractant are as follows: ethyl alcohol: nitric acid (selects the dense nitre that mass fraction is about 65%
Acid): water is mixed by 200mL:0.5mL:1000mL;
The actual conditions of ion chromatography described in step (2) are as follows: chromatographic column: CS12A analytical column is equipped with CG12A protection
Column;Flow velocity: 1.2mL/min;Sample volume: 100 μ L;Column temperature: 30 DEG C;Detection cell temperature: 35 DEG C;Detector: electric conductivity detector;Suppression
Device processed: CSRS-II;Suppressor electric current: 86mA;Elution program is shown in Table 1:
1. gradient elution program of table
Quantitative analysis described in step (3) uses external standard method, and the specific method is as follows:
A series of standard working solution for preparing reference substances containing various concentration object establishes standard using IC method
Working curve, the quantitative detection for sample;Cations in sample are calculated by formula (1) shown in Summary;
It the results are shown in Table 2:
2. assay result of table
Li in the sample of packaging bag containing cigarette can be detected simultaneously from can be seen that this method in table 2 and Fig. 2+、Na+、NH4+、
K+、Mg2+、Ca2+Deng 6 kinds of cations, and Gradient program elution cationic peak separating degree each compared with Gradient elution is more preferable, detects base
Line is more smooth, and detection limit is low.In addition, this method pre-treating method is simple, significantly simplifies sample preparation procedure, inspection is improved
Survey efficiency.
Li in 3 sample of packaging bag containing cigarette of embodiment+、Na+、NH4 +、K+、Mg2+、Ca2+Determination of ion content
(1) preparation of testing sample solution;
(2) it is detected using ion chromatography;
(3) quantitative analysis;
The specific method of step (1), (2) and (3) is same as Example 2, the difference is that step (1) was prepared
Testing sample solution is detected again after placing 12hr, and specific testing result is shown in Table 3,
3. assay result of table
As can be seen from Table 3, the testing result after testing sample solution placement 12hr and embodiment 2 detect immediately
As a result almost consistent, this illustrates, the Li in sample to be tested+、Na+、 NH4+、K+、Mg2+、Ca2+Protective effect of the ion in extractant
Under can be stabilized, content assaying method of the present invention extends the holding time of effective sample solution, greatly mentions
High daily sample amount detection.
Li in 4 sample of packaging bag containing cigarette of embodiment+、Na+、NH4 +、K+、Mg2+、Ca2+Determination of ion content
(1) preparation of testing sample solution;
(2) it is detected using ion chromatography;
(3) quantitative analysis;
The specific method of step (1), (2) and (3) is same as Example 2, the difference is that step (1) was prepared
Testing sample solution is detected again after placing r for 24 hours, and specific testing result is shown in Table 4:
4. assay result of table
As can be seen from Table 4, testing sample solution places what the testing result after r and embodiment 2 for 24 hours detected immediately
As a result almost consistent, this illustrates, the Li in sample to be tested+、Na+、 NH4+、K+、Mg2+、Ca2+Protective effect of the ion in extractant
Under can be stabilized, content assaying method of the present invention extends the holding time of effective sample solution, greatly mentions
High daily sample amount detection.
Li in 5 sample of packaging bag containing cigarette of embodiment+、Na+、NH4 +、K+、Mg2+、Ca2+Determination of ion content
(1) preparation of testing sample solution;
(2) it is detected using ion chromatography;
(3) quantitative analysis;
Step (1), (2), the specific method of (3) are same as Example 4, the difference is that the extractant in step (1)
Composition it is different.Specific testing result is shown in Table 5.
The composition of extractant are as follows: paraformaldehyde: ethyl alcohol: nitric acid (selects the concentrated nitric acid that mass fraction is about 65%): water is pressed
0.3g:400mL:10mL:1000mL mixing;
5. assay result of table
As can be seen from Table 5, the result of the detection of the testing result Yu embodiment 4 of testing sample solution almost one
It causes, this explanation, the Li in sample to be tested+、Na+、NH4+、K+、Mg2+、 Ca2+Ion is in the extraction using paraformaldehyde as stabilizer
It can be equally stabilized under the protective effect of agent, content assaying method of the present invention extends the guarantor of effective sample solution
The time is deposited, daily sample amount detection is greatly increased.
Although above having used general explanation and specific embodiment, the present invention is described in detail, at this
On the basis of invention, it can be made some modifications or improvements, this will be apparent to those skilled in the art.Therefore,
These modifications or improvements without departing from theon the basis of the spirit of the present invention are fallen within the scope of the claimed invention.
Claims (7)
1. Li in a kind of packaging bag containing cigarette+、Na+、NH4 +、K+、Mg2+、Ca2+The content assaying method of ion, which is characterized in that packet
Containing following steps:
(1) preparation of testing sample solution;
(2) it is detected using ion chromatography;
The preparation of testing sample solution described in step (1) method particularly includes: will contain after cigarette packaging bag extracts with extractant, extraction
Take liquid filter membrane to get the testing sample solution;The composition of the extractant are as follows: paraformaldehyde: ethyl alcohol: mass fraction
About 65% concentrated nitric acid: water is mixed, the tool of ion chromatography described in step (2) by 0.3g:400mL:10mL:1000mL
Body testing conditions are as follows: chromatographic column selects CS12A;Suppressor selects CSRS-II;Flow velocity is 1.2mL/min;Sample volume is 100 μ L;
Column temperature is 30 DEG C;Detection cell temperature is 35 DEG C;Detector: electric conductivity detector;Suppressor electric current is 86mA;Gradient is
0.001-0.035mol/L Loprazolam (MAS) isocratic elution or gradient elution program.
2. content assaying method according to claim 1, which is characterized in that testing sample solution described in step (1)
Preparation method particularly includes:
Cigarette packaging bag will be contained to be placed in collection vessel, be added extractant, ultrasound or oscillation extraction after, extract liquor filter membrane to get
The testing sample solution;The collection vessel selects the container made of acid-fast alkali-proof plastics.
3. content assaying method according to claim 2, which is characterized in that the acid-fast alkali-proof plastics be polyethylene or
Polytetrafluoroethylene (PTFE).
4. content assaying method according to claim 1 or 2, which is characterized in that the packaging bag containing cigarette and extractant
Amount ratio be 0.01-5g:5-100mL, extraction time 10-60min places 0-10min after extraction.
5. content assaying method according to claim 1 or 2, which is characterized in that the extract liquor filter membrane is using hole
Diameter 0.22 or 0.45 μm of filter membrane carry out, filter membrane material selection polyether sulfone (PES) filter membrane, hydrophilic Kynoar (PVDF) filter
Film or nylon66 fiber filter membrane.
6. content assaying method according to claim 1, which is characterized in that gradient elution program described in step (2)
Are as follows: when 0min, the concentration of Loprazolam is 18.0mmol/L;When 14.0min, the concentration of Loprazolam is 18.0mmol/L;
14.1min when, the concentration of Loprazolam is 24.0mmol/L;When 18.0min, the concentration of Loprazolam is 24.0mmol/L;
When 18.1min, the concentration of Loprazolam is 18.0mmol/L;When 20.0min, the concentration of Loprazolam is 18.0mmol/L.
7. content assaying method according to claim 1, which is characterized in that further include quantitative analysis step, described determines
Amount analysis uses external standard method or internal standard method.
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