CN105606757B - Sweetener and preservative method for measuring simultaneously in flavouring essence for tobacco - Google Patents
Sweetener and preservative method for measuring simultaneously in flavouring essence for tobacco Download PDFInfo
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- CN105606757B CN105606757B CN201610054607.7A CN201610054607A CN105606757B CN 105606757 B CN105606757 B CN 105606757B CN 201610054607 A CN201610054607 A CN 201610054607A CN 105606757 B CN105606757 B CN 105606757B
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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
- G01N30/96—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 using ion-exchange
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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
- G01N30/96—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 using ion-exchange
- G01N2030/965—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 using ion-exchange suppressor columns
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Abstract
The invention discloses sweetener in a kind of flavouring essence for tobacco and preservative method for measuring simultaneously, belong to cigarette auxiliary material chemical composition detection technique field.This method comprises the following steps：1) testing sample is taken to dilute, and it is 9~10 to adjust solution ph, extraction, extract crosses Oasis HLB column purifications, and filtering is standby；2) filtrate is taken to carry out ion chromatography, the content of sweetener and preservative in testing sample is calculated in reference standard curve.Physicochemical property of the invention according to different type flavouring essence for tobacco, classified purified removes the impurity of interference measurement in essence, and single injected sampling is carried out to 3 kinds of sweeteners (honey element, acesulfame potassium, saccharin sodium) in sample and 2 kinds of preservatives (sorbic acid, benzoic acid) using AS17C analytical columns and electric conductivity detector, separation determination simultaneously, the assay method of industry recommendation is compared, this method has the advantages that the range of linearity is wide, quantitative limit is low, sampling amount is few, determination efficiency is high.
Description
Technical field
The present invention relates to sweetener in a kind of flavouring essence for tobacco and preservative method for measuring simultaneously, belongs to cigarette auxiliary material chemistry
Composition detection technical field.
Background technology
2011, the problem of health ministry, Ministry of Agriculture etc. in Risk Monitoring and random checking according to finding, disclose
Illegal additive list in 151 kinds of food and feed, including 47 kinds may in food " the non-edible thing of illegal addition
Matter ", 22 kinds " easily abusing food additives " and 82 kinds " are forbidden eating in feed, animal drinking water and beasts, birds and aquatic products breeding process
Medicine and material ".Sorbic acid, honey element, benzoic acid, acesulfame potassium and saccharin sodium are in 151 kinds of illegal additive lists
" easily abusing food additives ", GB2760-2014《Food additives use standard》There is strict regulation to its addition.
Flavouring essence for tobacco has synthetic perfume and natural extract etc., and its chemical composition is mainly sugar, the compound such as alcohol, ester.Close
The perfuming of reason improves humectation and improves flammability etc. and play an important role for improving or improving the fragrance of cigarette.
For traditional cigarette sample, consumer mainly sucks sample by flue gas, and flavouring essence for tobacco does not directly act on
Consumer, but for novel tobacco product such as buccal cigarette, designer needs to take into account the mouthfeel of product, by adding one in essence
Quantitative sweetener, the jealous of buccal cigarette can be improved.In addition, many flavouring essence for tobaccos are natural extracts, for it is mould proof lose it is rotten,
Preservative can be added and extend storage life.While people consume buccal cigarette, these additives in essence will be straight by oral cavity
Tap into human body, it is therefore necessary to which Accurate Determining is carried out to its content.
Measure about sweetener in food and preservative, it has been reported that method have TLC, liquid chromatography,
GC-MS, the chromatography of ions and liquid chromatography tandem mass spectrometry etc..Tobacco business is on preservative in flavouring essence for tobacco
The measure of (sorbic acid, benzoic acid etc.) and sweetener (honey element) recommends liquid chromatography and the chromatography of ions.Acesulfame potassium and sugar
The measure of smart both sweeteners of sodium is temporarily recommended without correlation technique.In real work, a variety of sweeteners and anti-corrosion in flavouring essence for tobacco
The common measure of agent uses liquid chromatography more, but honey element (sodium cyclohexylsulfamate) measure it is less apply liquid phase, it is main
If because honey element is not absorbed in the range of ultraviolet-visible, column front derivation must be carried out before being determined using efficient liquid phase,
Operate Accurate Determining that is relatively complicated, while being not easy to realize Multiple components.
Liquid chromatography detects sweetener and preservative uses UV-detector, and the quantitative limit of each composition is all higher than 0.3 μ
G/mL, but Multiple components add simultaneously in actual sample, and the content of some compositions may be relatively low, near quantitative limit or low
In quantitative limit, the Accurate Determining of all the components will be difficult in this case.For example, professional standard measure honey element uses
AS11HC analytical columns, can be by the baseline separation of honey element and other ions by the gentle eluent concentration of adjustable column, but marks
The range of linearity of directrix curve is only suitable for the measure that concentration is more than 10 μ g/mL samples, and AS11HC analytical columns are to acesulfame potassium, saccharin
Both strong reservation ion elutions of sodium are still more difficult.
The content of the invention
It is an object of the invention to provide sweetener in a kind of flavouring essence for tobacco and preservative method for measuring simultaneously.
In order to realize the above object the technical solution adopted in the present invention is：
Sweetener and preservative method for measuring simultaneously, comprise the following steps in flavouring essence for tobacco：
1) testing sample is taken to dilute, and it is 9~10 to adjust solution ph, extraction, extract crosses Oasis HLB column purifications,
Filter standby；
2) filtrate is taken to carry out ion chromatography, sweetener and preservative in testing sample is calculated in reference standard curve
Content.
The sweetener is the one or more in honey element, acesulfame potassium, saccharin sodium.
The preservative is sorb acids (sorbic acid and its salt) and/or benzoic acids (benzoic acid and its salt).
Testing sample is aqueous samples or water-insoluble sample in step 1), and aqueous samples can directly be diluted with water,
Again with NaOH adjust solution ph, after sample is extracted by high-speed homogenization method (extract, such as rotating speed 8000~
1~2min of homogenate extraction under 12000rpm), extract is that clear liquid can directly cross Oasis HLB column purifications；For water-insoluble sample
Product are, it is necessary to which first with the mixed liquor of water and alcohol, (alcohol is short chain alcohol, C1~C4, the volume of methanol or ethanol, alcohol and water specifically may be selected
Than for 1:3~4) dilute, then with NaOH adjust solution ph, after pass through high-speed homogenization method (8000~12000rpm of rotating speed) extract
Sample, when extract is clear liquid, Oasis HLB column purifications can be directly crossed, when extract is suspension, supercentrifuge need to be used
Further separation, supernatant is taken to cross the analysis of Oasis HLB column purifications.
Oasis HLB posts can remove the organic impurities in sample in step 1), with lipophilicity divinylbenzene and hydrophily N-
The macroporous copolymer that vinylpyrrolidone monomer forms by a certain percentage is filler, compares C18Post, the surface of HLB post adsorbents
Product is big, and capacity is about C183 times of post, purification efficiency is higher.
The filter membrane that filtering uses in step 1) should select according to liquid to be filtered property.When testing sample is aqueous samples
When, when diluent uses water, filter membrane selects water system filter membrane, such as polyether sulfone or the acetyl cellulose filter in 0.45 μm of aperture
Film；When testing sample is water-insoluble sample, diluent need to select organic system filter membrane using alcohol and the mixed liquor of water, filter membrane,
Such as 0.22 μm of the nylon leaching film in aperture.
The chromatography of step 2) intermediate ion uses DIONEX ICS3000 type ion chromatographs, and detector is Conductivity detection
Device, chromatographic condition are：Anion analysis post IonPac AS17C, specification 4mm × 250mm；Guard column IonPac AG17C, specification
4mm×50mm；Leacheate is KOH solution, gradient elution, gradient condition：0.0~13.0min 5mmol/L, 13.1~
23.0min 70mmol/L, 23.1~30.0min 5mmol/L, system flow rate 0.8mL/min；Suppress electric current 174mA, sample introduction
Measure 25 μ L, acquisition time 30min.
The preparation method of step 2) standard curve is：The standard substance of sweetener and preservative is taken to be configured to series concentration
Mixed standard solution, regression analysis is made with peak area tie substance concentration after ion chromatography, obtain material concentration with
The relation curve of peak area.
Beneficial effects of the present invention：
The anion base of easily ionizable is all carried in this 5 kinds of molecules of sorbic acid, honey element, benzoic acid, acesulfame potassium, saccharin sodium
Group, therefore ion chromatography method can be selected, pass through the content of 5 kinds of compositions in anion exchange separation simultaneously determination sample.This
According to the physicochemical property of different type flavouring essence for tobacco, classified purified removes the impurity of interference measurement in essence, and uses for invention
AS17C analytical columns and electric conductivity detector carry out single injected sampling, while separation determination to 3 kinds of sweeteners in sample and 2 kinds of preservatives.
The range of linearity of the assay method is wider, it is possible to achieve sorbic acid, honey element, benzoic acid, acesulfame potassium, saccharin sodium are in 0.1~10 μ
Assay in the range of g/mL, the assay method of industry recommendation is compared, the quantitative limit of this method is lower (the μ g/mL of ＜ 0.2), takes
Sample amount is less, can meet the detection demand of low content composition, while determination efficiency is high, while 5 kinds of compositions can be achieved in 30min
Measure.
3 kinds are weak reservation ion in above-mentioned 5 kinds of molecules, and 2 kinds retain ion to be strong, and retention properties difference is notable, using two
Rank isoconcentration leacheate, high concentration is immediately switched to after the completion of low concentration elution, analysis time can be saved to greatest extent, and
Stable baseline and good peak shape are obtained in two ranks are analyzed.
Brief description of the drawings
Fig. 1 is the chromatography of ions figure of mixed standard solution 6 in embodiment 1；
Fig. 2 is the chromatography of ions figure of aqueous samples in embodiment 1；
Fig. 3 is the chromatography of ions figure of water-insoluble sample in embodiment 2.
Embodiment
Following embodiments are only described in further detail to the present invention, but do not form any limitation of the invention.
Embodiment 1
Sweetener and preservative method for measuring simultaneously, comprise the following steps in flavouring essence for tobacco (aqueous samples)：
1) sample pre-treatments
0.1232g samples accurately are weighed into 50mL conical flask with stopper, add water 50mL, and adjust solution ph with NaOH
9.5, high-speed homogenization (rotating speed 10000rpm) extraction 1.5min, purification (is activated) through 3mL methanol and 3mL water through Oasis HLB posts
After (flow velocity ＜ 1.0mL/min), 0.45 μm of polyethersulfone membranes is crossed, discards former milliliters of filtrates, subsequent filtrate is to be measured after collection；
2) mixed standard solution is prepared
The mixed standard solution of series concentration is prepared using pH 9.5 NaOH solution, the specific concentration of standard substance is seen below
Table 1；
The mixed standard solution concentration table of table 1
According to GB2760-2014, this 5 kinds of material limitations of honey element, acesulfame potassium, saccharin sodium, sorbic acid, benzoic acid are with food
Type it is otherwise varied, but overall limitation scope is between 0.1~5g/kg.When testing sample 0.1~0.2g of sampling amount, dilution
During 40~50 times of multiple, standard curve needs the measure of the μ g/mL content samples of covering 0.2~10, and above-mentioned standard curve ranges
For 0.1~10 μ g/mL, it can meet that this 5 kinds of materials of honey element, acesulfame potassium, saccharin sodium, sorbic acid, benzoic acid allow addition
Measure requirement, and relative to the measure of honey element in industry recommendation method, standard curve determination scope reduces by 10 times；Separately
Outside, the maximum concentration of each composition should be less than 10 μ g/mL in mixed standard solution, because AS17C column packing matrix is non-porous
EVB-DVB polymer, selectivity is high, is adapted to complex system sample analysis, and the ion exchanging function radix amount of unit volume is few,
Under 25 μ L sampling condition, the composition peak type to be measured higher than this concentration can trail, and this also from illustrating this analysis on the other hand
Post is adapted to the measure of low content sample, can be by dilution (or improving extract volume) come real for the higher composition of content
Now determine, relative to liquid chromatogram sampling amount, it is necessary to sample size it is less.
3) standard curve is made
Mixed standard solution is taken to carry out ion chromatography, using DIONEX ICS3000 types ion chromatograph (with elution
Liquid generator), electric conductivity detector, chromatographic condition is：Anion analysis post IonPac AS17C, specification 4mm × 250mm, protection
Post IonPac AG17C, specification 4mm × 50mm, leacheate are KOH solution, gradient elution (elution requirement see the table below 2), system stream
Speed is 0.8mL/min；Suppress electric current 174mA, sample size 25 μ L, acquisition time 30min；Fig. 1 show mixed standard solution 6
Chromatography of ions figure, wherein 1~5 represents the peak of sorbic acid, honey element, benzoic acid, acesulfame potassium, saccharin sodium successively；
The condition of gradient elution of table 2
Instrument setting program end of run, integral condition, peak area quantification qualitative with retention time, according to peak face are set
Product makees regression analysis to its respective concentration, obtains a curve of material concentration and peak area, linear equation and coefficient correlation are shown in
Table 3 below, wherein y are peak area (μ Smin), and x is the mass concentration (μ g/mL) of each composition in testing sample.
The standard curve and coefficient correlation of the standard substance of table 3
The detection limit (LOD) and quantitative limit (LOQ) of each composition are made with the mixed standard solution of least concentration (0.1 μ g/mL)
Unknown sample, repeat sample introduction 10 times, standard deviation counted by the concentration value measured, LOD is tried to achieve with 3 times of standard deviations, LOQ with
10 times of standard deviations are tried to achieve, and the detection limit and quantitative limit of above-mentioned 5 kinds of composition measurements see the table below 4.
The detection limit and quantitative limit (μ g/mL) of 45 kinds of compositions of table
From table 4, it can be seen that the quantitative limit of 5 kinds of compositions is up to 0.310 μ g/mL, liquid chromatogram and chromatography of ions are compared
AS11HC analytical column assay methods, quantitative limit is lower, and the detection for being especially suitable for micro constitutent judges.
4) sample analysis determines
Filtrate in step 1) is taken to carry out ion chromatography, using DIONEX ICS3000 types ion chromatograph (with elution
Liquid generator), electric conductivity detector, chromatographic condition is same as above, and the chromatography of ions figure for detecting sample is shown in Fig. 2, wherein 1,2 represent mountain successively
Pears acid, the peak of benzoic acid；By detecting the peak area of sample, the concentration as corresponding to standard curve obtains sample, i.e. Instrument observation
Value, the content that composition is detected in sample is calculated according still further to following formula 1；
Formula 1：
In formula, X：The Instrument observation value of sample, unit are micrograms per millilitre (μ g/mL), V：Extract volume, unit are milli
Rise (mL), m：Sample quality, unit are gram (g)；
Only have sorbic acid and benzoic acid there are data in the observation that this sample obtains, other compositions do not detect, public more than
Formula calculates sorbic acid in sample, the content of benzoic acid is respectively 1.43g/kg, 1.02g/kg.
Embodiment 2
Sweetener and preservative method for measuring simultaneously, comprise the following steps in flavouring essence for tobacco (water-insoluble sample)：
1) sample pre-treatments
0.1009g samples accurately are weighed into 50mL conical flask with stopper, add 1:3 (v/v) methanol aqueous solution 50mL, use
NaOH regulation solution ph is 9.5, and high-speed homogenization (rotating speed 10000rpm) extraction 1.5min, extraction, which finishes, moves to solution at a high speed
Centrifuge (rotating speed 16000rpm) separates 1min, takes supernatant (to be activated through Oasis HLB posts through 3mL methanol and 3mL water)
After purifying (flow velocity ＜ 1.0mL/min), 0.22 μm of nylon leaching film is crossed, discards former milliliters of filtrates, subsequent filtrate is to be measured after collection；
2) mixed standard solution preparation and standard curve making are the same as embodiment 1；
3) sample analysis determines
Filtrate in step 1) is taken to carry out ion chromatography, using DIONEX ICS3000 types ion chromatograph (with elution
Liquid generator), electric conductivity detector, for chromatographic condition with embodiment 1, the chromatography of ions figure for detecting sample is shown in Fig. 3, wherein 1~3 successively
Represent the peak of sorbic acid, honey element, acesulfame potassium；It is dense as corresponding to standard curve obtains sample by detecting the peak area of sample
Degree, i.e. Instrument observation value, the content that composition is detected in sample is calculated according still further to equation 1 above；
Only have sorbic acid, honey element and acesulfame potassium there are data in the observation that this sample obtains, other compositions do not detect, by
It is respectively 0.73g/kg, 18g/kg, 1.01g/kg that formula 1, which calculates sorbic acid in sample, honey element, the content of acesulfame potassium,.
Test example
1) the precision test of Ion Chromatographic Method
Water-soluble and water-insoluble blank sample respectively, honey element containing finite concentration, acesulfame potassium, saccharin are added thereto
The mixed standard solution of sodium, sorbic acid and benzoic acid, it is well mixed, obtains testing positive used, refer again to embodiment 1
In~2 in method measure positive 5 kinds of compositions content, each sample replication 5 times, the precision of method of testing, knot
Fruit see the table below 5.
The precision test result of the different type sample of table 5
As can be seen from Table 5, although 2 type sample Pretreatments are different, 5 kinds of measure compositions in sample
Relative mean standard deviation within 10%, illustrate that the precision of this method is good, can meet measure require.
2) recovery of standard addition is tested
The mixed standard solution that a certain amount of high, medium and low concentration is added in above-mentioned water-soluble and water-insoluble sample (is seen below
Table 6), with reference to method in embodiment 1~3,5 kinds of honey element, acesulfame potassium, saccharin sodium, sorbic acid, benzoic acid compositions in determination sample
Content, as a result see the table below 6.
The mark-on reclaims test result of the different type sample of table 6
As can be seen from Table 6, in 2 type samples 5 kinds measure composition recovery of standard addition 94.3%~100.5%
Between, illustrate that the degree of accuracy of this method is good, can meet that measure requires.
Claims (5)
1. sweetener and preservative method for measuring simultaneously in flavouring essence for tobacco, it is characterised in that：Comprise the following steps：
1) testing sample is taken to dilute, and it is 9~10 to adjust solution ph, extraction, extract crosses Oasis HLB column purifications, filters
It is standby；
2) filtrate is taken to carry out ion chromatography, containing for sweetener and preservative in testing sample is calculated in reference standard curve
Amount；The condition of step 2) intermediate ion chromatography is：Anion analysis post IonPac AS17C, specification 4mm × 250mm；Protection
Post IonPac AG17C, specification 4mm × 50mm；Leacheate is KOH solution, gradient elution, gradient condition：0.0~13.0min
5mmol/L, 13.1~23.0min 70mmol/L, 23.1~30.0min 5mmol/L, system flow rate 0.8mL/min；Suppress
Electric current 174mA, sample size 25 μ L, acquisition time 30min；
Testing sample is aqueous samples or water-insoluble sample in step 1), and aqueous samples are using water as diluent, water
Insoluble sample is using the mixed liquor of short chain alcohol and water as diluent；The sweetener is honey element, acesulfame potassium and saccharin sodium；
The preservative is sorbic acid and benzoic acid.
2. according to the method for claim 1, it is characterised in that：The extraction is to be homogenized under 8000~12000rpm of rotating speed
Extract 1~2min.
3. according to the method for claim 1, it is characterised in that：During using water as diluent, filter membrane selects water system filter membrane；
During using the mixed liquor of short chain alcohol and water as diluent, filter membrane selects organic system filter membrane.
4. according to the method for claim 1, it is characterised in that：The chromatography of step 2) intermediate ion uses DIONEX
ICS3000 type ion chromatographs, detector are electric conductivity detector.
5. according to the method for claim 1, it is characterised in that：The preparation method of step 2) standard curve is：Take sweet taste
The standard substance of agent and preservative is configured to the mixed standard solution of series concentration, corresponding with peak area after ion chromatography
Material concentration makees regression analysis, obtains the relation curve of material concentration and peak area.
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| CN107037174B (en) * | 2016-11-29 | 2018-11-13 | 赵会宇 | The assay method of the residual quantity of acesulfame potassium in hawthorn |
| CN106556660A (en) * | 2016-11-29 | 2017-04-05 | 赵会宇 | The assay method of the residual quantity of cyclamate in Fructus Persicae |
| CN106706800A (en) * | 2017-02-15 | 2017-05-24 | 英格尔检测技术服务（青岛）有限公司 | Method for rapidly detecting benzoic acid, sorbic acid, sodium saccharin and acesulfame potassium |
| CN107365627B (en) * | 2017-06-09 | 2020-09-22 | 广东中烟工业有限责任公司 | Additive for prolonging quality guarantee period of tobacco flavor |
| CN107367558B (en) * | 2017-07-06 | 2019-08-06 | 山东天元盈康检测评价技术有限公司 | A kind of ion detection method of p-aminobenzoic acid |
| CN108680689A (en) * | 2018-05-11 | 2018-10-19 | 大连市食品检验所 | A kind of method of Advantest sweet tea in measurement food |
| CN108872448B (en) * | 2018-09-18 | 2020-09-22 | 国家烟草质量监督检验中心 | Method for detecting 5 sweetening agents in tobacco essence by ultra-high performance liquid chromatography-tandem mass spectrometry |
| CN108956840B (en) * | 2018-09-18 | 2021-01-26 | 国家烟草质量监督检验中心 | Method for detecting 5 sweetening agents in electronic cigarette liquid through ultra-high performance liquid chromatography-tandem mass spectrometry |
| CN108776187B (en) * | 2018-09-18 | 2020-09-29 | 国家烟草质量监督检验中心 | Method for detecting 5 sweetening agents in tipping paper for cigarettes by ultra-high performance liquid chromatography-tandem mass spectrometry |
| CN110763797B (en) * | 2019-11-12 | 2022-04-19 | 河南中烟工业有限责任公司 | Method for measuring sweetening agent for cigarettes by high performance liquid chromatography |
| CN112649528A (en) * | 2020-12-14 | 2021-04-13 | 安徽中青检验检测有限公司 | Food preservative content safety detection method |
| CN114778726A (en) * | 2022-04-19 | 2022-07-22 | 湘潭市食品药品检验所 | Detection method for simultaneously measuring four additives in flour product |
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| US9084439B2 (en) * | 2011-09-22 | 2015-07-21 | R.J. Reynolds Tobacco Company | Translucent smokeless tobacco product |
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| CN104614466B (en) * | 2015-02-16 | 2016-04-06 | 国家烟草质量监督检验中心 | The assay method of antiseptic in tobacco juice for electronic smoke |
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