CN105606757A - Method for simultaneously determining sweetening agents and preservatives in tobacco essence - Google Patents
Method for simultaneously determining sweetening agents and preservatives in tobacco essence Download PDFInfo
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- G—PHYSICS
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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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Abstract
The invention discloses a method for simultaneously determining sweetening agents and preservatives in tobacco essence, and belongs to the technical field of chemical component detection of auxiliary materials for tobaccos. The method comprises the following steps that 1, a sample to be determined is diluted, the pH value of a solution is regulated to be 9-10, extraction is performed, extraction liquid is purified through an Oasis HLB column, and the purified extraction liquid is filtered for standby application; 2, filtrate is taken to be subjected to ion chromatographic analysis, and the content of the sweetening agents and the preservatives in the sample to be determined is calculated by contrasting a standard curve. According to the method, impurities disturbing determination in the essence are purified and removed in a classifying mode according to the physical and chemical properties of different types of the tobacco essence, one-time sample feeding is performed on the three sweetening agents (sodium cyclamate, acesulfame and saccharin sodium) and the two preservatives (sorbic acid and benzoic acid) through an AS17C analytical column and an electrical conductivity detector, and separation and determination are simultaneously performed. Compared with an industrially recommended determination method, the method has the advantages of being wide in linear range, low in quantitation limit, little in sampling quantity, high in determination efficiency and the like.
Description
Technical field
The present invention relates to sweetener and anticorrisive agent method for measuring simultaneously in a kind of flavouring essence for tobacco, belong to cigarette auxiliary material chemical compositionDetection technique field.
Background technology
2011, health ministry, the Ministry of Agriculture etc., according to the problem of finding in Risk Monitoring and random checking, announced 151The illegal material list that adds in kind of food and feed, comprising 47 kinds may be in food " the non-edible thing of illegal interpolationMatter ", 22 kinds " easily abusing food additives " and 82 kinds " forbid at feed, animal drinking water and beasts, birds and aquatic products breeding processIn edible medicine and material ". Sorbic acid, honey element, benzoic acid, acesulfame potassium and saccharin sodium are 151 kinds of illegal additives" easily abusing food additives " in list, GB2760-2014 " food additives use standard " has strictly its additionRegulation.
Flavouring essence for tobacco has synthetic perfume and natural extract etc., and its chemical composition is mainly sugar, alcohol, the compounds such as ester. RationallyPerfuming for improving or improve the fragrance of cigarette, improve humectation and improve flammability etc. and play an important role.
For traditional cigarette sample, consumer mainly sucks sample by flue gas, and flavouring essence for tobacco is not to directly act on consumptionPerson, but for novel tobacco goods as sucked cigarette, designer need to take into account the mouthfeel of product, certain by adding in essenceThe sweetener of amount, can improve and suck the jealous of cigarette. In addition, many flavouring essence for tobaccos are natural extracts, for mildew-resistant lose rotten,Can add anticorrisive agent and extend storage life. When cigarette is sucked in people's consumption, these additives in essence will be straight by oral cavityTap into into human body, be therefore necessary its content to carry out Accurate Determining.
The mensuration of sweetener and anticorrisive agent in related food, the method for having reported has TLC, liquid chromatography, gasPhase chromatogram mass spectrography, the chromatography of ions and Liquid Chromatography-Tandem Mass Spectrometry method etc. Tobacco business is about anticorrisive agent (mountain in flavouring essence for tobaccoPears acid, benzoic acid etc.) and the mensuration of sweetener (honey element) recommend liquid chromatography and the chromatography of ions. Acesulfame potassium and sugarThe mensuration of these two kinds of sweeteners of essence sodium is recommended without correlation technique temporarily. In real work, multiple sweetener and anticorrosion in flavouring essence for tobaccoThe common mensuration of agent adopts liquid chromatography more, but the less application liquid phase of the mensuration of honey element (sodium cyclohexylsulfamate),Be mainly because honey element is not absorbed in UV, visible light optical range, employing high efficiency liquid phase must carry out spreading out before post before measuringRaw, operate comparatively loaded down with trivial detailsly, the while is also difficult for realizing the Accurate Determining of Multiple components.
Liquid chromatography detects sweetener and anticorrisive agent all adopts UV-detector, and the quantitative limit of each composition is all greater than0.3 μ g/mL, but in actual sample, Multiple components adds simultaneously, and the content of some composition may be on the low side, near quantitative limitOr lower than quantitative limit, the Accurate Determining of all the components will be difficult to realize in this case. For example, professional standard is measured sweetHoney element adopts AS11HC analytical column, the baseline of honey element and other ions can be divided by the gentle eluent concentration of adjustable columnFrom, but the range of linearity of calibration curve is only suitable for the mensuration that concentration is greater than 10 μ g/mL samples, and AS11HC analytical columnThese two kinds strong of acesulfame potassiums, saccharin sodium are retained to still difficulty comparatively of ion wash-outs.
Summary of the invention
The object of this invention is to provide sweetener and anticorrisive agent method for measuring simultaneously in a kind of flavouring essence for tobacco.
In order to realize above object, the technical solution adopted in the present invention is:
Sweetener and anticorrisive agent method for measuring simultaneously in flavouring essence for tobacco, comprises the following steps:
1) get testing sample dilution, and regulator solution pH value is 9～10, extracts, extract is crossed OasisHLB column purification,Filter for subsequent use;
2) get filtrate and carry out ion chromatography, reference standard curve calculation obtains sweetener and anticorrisive agent in testing sampleContent.
Described sweetener is one or more in honey element, acesulfame potassium, saccharin sodium.
Described anticorrisive agent is sorb acids (sorbic acid and salt thereof) and/or benzoic acids (benzoic acid and salt thereof).
Step 1) in testing sample be water-soluble sample or water-insoluble sample, water-soluble sample is dilute with water directly, thenBy NaOH regulator solution pH value, after by high-speed homogenization method, sample is extracted that (i.e. extraction, as at rotating speedUnder 8000～12000rpm, 1～2min is extracted in homogenate), extract is that clear liquid can be direct be crossed OasisHLB column purification; For waterInsoluble sample, need first water and alcohol mixed liquor (alcohol is short chain alcohol, and C1～C4 specifically can select methyl alcohol or ethanol,The volume ratio of alcohol and water is 1:3～4) dilution, then by NaOH regulator solution pH value, afterwards by high-speed homogenization method (rotating speed8000～12000rpm) extraction sample, when extract is clear liquid, can directly cross OasisHLB column purification, extract is for outstandingWhen turbid liquid, need to adopt supercentrifuge further to separate, get supernatant and cross the analysis of OasisHLB column purification.
Step 1) in OasisHLB post can remove the organic impurities in sample, with lipophilicity divinylbenzene and hydrophily N-secondThe macroporous copolymer that thiazolinyl pyrrolidones monomer forms is by a certain percentage filler, compares C18Post, the table of HLB post adsorbentArea is large, and capacity is about C183 times of post, purification efficiency is higher.
Step 1) in filter adopt filter membrane should select according to liquid to be filtered character. In the time that testing sample is water-soluble sample,When diluent adopts water, filter membrane is selected water system filter membrane, as the polyether sulfone of aperture 0.45 μ m or acetyl cellulose filter membrane;In the time that testing sample is water-insoluble sample, diluent adopts the mixed liquor of alcohol and water, and filter membrane need be selected organic system filter membrane, asThe nylon leaching film of aperture 0.22 μ m.
Step 2) intermediate ion chromatography employing DIONEXICS3000 type ion chromatograph, detector is electric conductivity detector,Chromatographic condition is: anion analysis post IonPacAS17C, specification 4mm × 250mm; Guard column IonPacAG17C, ruleLattice 4mm × 50mm; Leacheate is KOH solution, gradient elution, and gradient condition: 0.0～13.0min5mmol/L,13.1～23.0min70mmol/L, 23.1～30.0min5mmol/L, system flow rate is 0.8mL/min; Suppress electric current 174mA,Sample size 25 μ L, acquisition time 30min.
Step 2) preparation method of Plays curve is: the standard substance of getting sweetener and anticorrisive agent is mixed with series concentrationMixed standard solution is done regression analysis with peak area tie substance concentration after ion chromatography, obtains material concentration and peakThe relation curve of area.
Beneficial effect of the present invention:
Anionic group with easily ionizable all in sorbic acid, honey element, benzoic acid, acesulfame potassium, these 5 kinds of molecules of saccharin sodium,Therefore can select ion chromatography method, by the content of 5 kinds of compositions in anion exchange separation while working sample. ThisBright according to the physicochemical property of dissimilar flavouring essence for tobacco, classified purified is removed the impurity of interference measurement in essence, and adoptsAS17C analytical column and electric conductivity detector carry out single injected sampling to 3 kinds of sweeteners and 2 kinds of anticorrisive agents in sample, separate and survey simultaneouslyFixed. The range of linearity of this assay method is wider, can realize sorbic acid, honey element, benzoic acid, acesulfame potassium, saccharin sodium and existAssay within the scope of 0.1～10 μ g/mL, compares the assay method that industry is recommended, the lower (< of quantitative limit of the method0.2 μ g/mL), sampling amount still less, can meet the detection demand of low content composition, and determination efficiency is high simultaneously, can be real in 30minWhen existing 5 kinds of compositions, measure.
In above-mentioned 5 kinds of molecules, 3 kinds is weak reservation ion, and 2 kinds is the strong ion that retains, and retention properties difference significantly, adopts twoRank isoconcentration leacheate, is switched to high concentration after low concentration drip washing completes immediately, can save to greatest extent analysis time,And in analyzing, two rank obtain baseline and good peak shape stably.
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 water-soluble sample in embodiment 1;
Fig. 3 is the chromatography of ions figure of water-insoluble sample in embodiment 2.
Detailed description of the invention
Following embodiment is only described in further detail the present invention, but does not form any limitation of the invention.
Embodiment 1
Sweetener and anticorrisive agent method for measuring simultaneously in flavouring essence for tobacco (water-soluble sample), comprises the following steps:
1) sample pre-treatments
Accurately take 0.1232g sample to 50mL tool plug triangular flask, the 50mL that adds water, and with NaOH regulator solution pHValue 9.5, high-speed homogenization (rotating speed 10000rpm) extract 1.5min, through OasisHLB post (through 3mL methyl alcohol and 3mLWater activation) purify after (flow velocity < 1.0mL/min), cross 0.45 μ m polyether sulfone filter membrane, discard former milliliters of filtrates, collectRear subsequent filtrate is to be measured;
2) preparation mixed standard solution
The mixed standard solution that adopts the NaOH solution preparation series concentration of pH9.5, the concrete concentration of standard substance sees the following form1；
Table 1 mixed standard solution concentration table
According to GB2760-2014, honey element, acesulfame potassium, saccharin sodium, sorbic acid, these 5 kinds of materials of benzoic acid are limited the quantity with foodThe type of product is distinguished to some extent, but the scope of totally limiting the quantity is between 0.1～5g/kg. As testing sample sampling amount 0.1～0.2g, dilutionWhen 40～50 times of multiples, calibration curve need to cover the mensuration of 0.2～10 μ g/mL content sample, and above-mentioned standard curve rangeBe 0.1～10 μ g/mL, can meet honey element, acesulfame potassium, saccharin sodium, sorbic acid, these 5 kinds of materials of benzoic acid and allow to addThe mensuration requirement of dosage, and with respect to the mensuration of honey element in industry recommend method, standard curve determination scope reduces by 10Doubly; In addition, in mixed standard solution, the maximum concentration of each composition should be less than 10 μ g/mL, and this is because AS17C column packing baseMatter is the EVB-DVB polymer of atresia, selectively high, is applicable to complex system sample analysis, the ion-exchange of unit volumeFunction radix amount is few, under the sampling condition of 25 μ L, can trail higher than the one-tenth swarming type to be measured of this concentration, and this is also from anotherIndividual aspect illustrates that this analytical column is applicable to the mensuration of low content sample, for the higher composition of content, can (or carry by dilutionHigh extract volume) realize mensuration, with respect to the sampling amount of liquid chromatogram, the sample size needing is still less.
3) production standard curve
Get mixed standard solution and carry out ion chromatography, adopt DIONEXICS3000 type ion chromatograph (to join leacheateGenerator), electric conductivity detector, chromatographic condition is: anion analysis post IonPacAS17C, specification 4mm × 250mm,Guard column IonPacAG17C, specification 4mm × 50mm, leacheate is KOH solution, gradient elution is (under elution requirement is shown inTable 2), system flow rate is 0.8mL/min; Suppress electric current 174mA, sample size 25 μ L, acquisition time 30min; Fig. 1Be depicted as the chromatography of ions figure of mixed standard solution 6, wherein 1～5 represent successively sorbic acid, honey element, benzoic acid, An SaiThe peak of honey, saccharin sodium;
Table 2 condition of gradient elution
Instrument setting program end of run, arranges integral condition, qualitative with retention time, and peak area quantification, according to peak areaIts respective concentration is done to regression analysis, obtain a curve of material concentration and peak area, under linear equation and coefficient correlation are shown inTable 3, wherein y is peak area (μ Smin), x is the mass concentration (μ g/mL) of each composition in testing sample.
The calibration curve of table 3 standard substance and coefficient correlation
The detection limit (LOD) of each composition and the mixed standard solution of least concentration (0.1 μ g/mL) for quantitative limit (LOQ)Make unknown sample, repeat sample introduction 10 times, count standard deviation by the concentration value recording, LOD asks with 3 times of standard deviations, LOQ tries to achieve with 10 times of standard deviations, and the detection limit of above-mentioned 5 kinds of composition measurements and quantitative limit see the following form 4.
The detection limit of table 45 kind of composition and quantitative limit (μ g/mL)
As can be seen from Table 4, the quantitative limit of 5 kinds of compositions is up to 0.310 μ g/mL, compares liquid chromatogram and chromatography of ionsAS11HC analytical column assay method, quantitative limit is lower, and the detection that is applicable to very much micro constitutent is judged.
4) sample analysis is measured
Get step 1) in filtrate carry out ion chromatography, adopt DIONEXICS3000 type ion chromatograph (to join drip washingLiquid generator), electric conductivity detector, chromatographic condition is the same, and the chromatography of ions figure that detects sample is shown in Fig. 2, and wherein 1,2 successivelyRepresent sorbic acid, benzoic peak; By detecting the peak area of sample, obtain by calibration curve the concentration that sample is corresponding,Instrument observation value, then detect according to the following formula the content of composition in 1 calculation sample;
Formula 1:
In formula, X: the Instrument observation value of sample, unit is every milliliter of microgram (μ g/mL), V: extract volume, unit isMilliliter (mL), m: sample quality, unit is gram (g);
In the observation that this sample obtains, only have sorbic acid and benzoic acid to have data, other compositions do not detect, by above formula meterCalculate sorbic acid in sample, benzoic content is respectively 1.43g/kg, 1.02g/kg.
Embodiment 2
Sweetener and anticorrisive agent method for measuring simultaneously in flavouring essence for tobacco (water-insoluble sample), comprises the following steps:
1) sample pre-treatments
Accurately take 0.1009g sample to 50mL tool plug triangular flask, add 1:3 (v/v) methanol aqueous solution 50mL, useNaOH regulator solution pH value is 9.5, and high-speed homogenization (rotating speed 10000rpm) extracts 1.5min, extracts complete by solutionMove to supercentrifuge centrifugal (rotating speed 16000rpm) separate 1min, get supernatant through OasisHLB post (through 3mL firstAlcohol and the activation of 3mL water) purify after (flow velocity < 1.0mL/min), cross 0.22 μ m nylon leaching film, discard former milliliters of filtrates,After collecting, subsequent filtrate is to be measured;
2) mixed standard solution preparation and standard curve making are with embodiment 1;
3) sample analysis is measured
Get step 1) in filtrate carry out ion chromatography, adopt DIONEXICS3000 type ion chromatograph (to join drip washingLiquid generator), electric conductivity detector, chromatographic condition is with embodiment 1, and the chromatography of ions figure that detects sample is shown in Fig. 3, wherein 1～3Represent successively the peak of sorbic acid, honey element, acesulfame potassium; By detecting the peak area of sample, obtain sample pair by calibration curveThe concentration of answering, i.e. Instrument observation value, then according to the content that detects composition in above formula 1 calculation sample;
In the observation that this sample obtains, only have sorbic acid, honey element and acesulfame potassium to have data, other compositions do not detect, by formula1 content that calculates sorbic acid in sample, honey element, acesulfame potassium is respectively 0.73g/kg, 18g/kg, 1.01g/kg.
Test example
1) precision of Ion Chromatographic Method test
Fetch water respectively dissolubility and water-insoluble blank sample, add wherein containing finite concentration honey element, acesulfame potassium, saccharin sodium,Sorbic acid and benzoic mixed standard solution, mix, and obtains testing positive used, refers again to embodiment 1～2Middle method is measured the content of 5 kinds of compositions in positive, each sample replication 5 times, the precision of method of testing, knotFruit sees the following form 5.
The precision test result of the dissimilar sample of table 5
As can be seen from Table 5, although 2 types of sample Pretreatments are different, in sample, measure composition for 5 kindsRelative mean standard deviation all in 10%, illustrate that the precision of the method is good, can meet mensuration requirement.
2) recovery of standard addition test
In above-mentioned water-soluble and water-insoluble sample, add the mixed standard solution of a certain amount of high, medium and low concentration (to see the following form6), with reference to method in embodiment 1～3,5 kinds of honey elements in working sample, acesulfame potassium, saccharin sodium, sorbic acid, benzoic acidThe content of composition, the results are shown in following table 6.
The mark-on of the dissimilar sample of table 6 reclaims test result
As can be seen from Table 6, in 2 types of samples 5 kinds of recovery of standard addition of measuring compositions all between 94.3%～100.5%,The degree of accuracy that the method is described is good, can meet mensuration requirement.
Claims (10)
1. sweetener and anticorrisive agent method for measuring simultaneously in flavouring essence for tobacco, is characterized in that: comprise the following steps:
1) get testing sample dilution, and regulator solution pH value is 9～10, extracts, extract is crossed OasisHLB column purification,Filter for subsequent use;
2) get filtrate and carry out ion chromatography, reference standard curve calculation obtains sweetener and anticorrisive agent in testing sampleContent.
2. method according to claim 1, is characterized in that: described sweetener is honey element, acesulfame potassium, asccharinOne or more in sodium.
3. method according to claim 1, is characterized in that: described anticorrisive agent is sorb acids and/or benzoic acids.
4. method according to claim 3, is characterized in that: described anticorrisive agent is sorbic acid and/or benzoic acid.
5. method according to claim 1, is characterized in that: step 1) in testing sample be water-soluble sample or waterInsoluble sample, water-soluble sample adopts water as diluent, and water-insoluble sample adopts the mixed liquor conduct of short chain alcohol and waterDiluent.
6. method according to claim 1, is characterized in that: described extraction is under rotating speed 8000～12000rpm1～2min is extracted in homogenate.
7. method according to claim 5, is characterized in that: while adopting water as diluent, filter membrane is selected water systemFilter membrane; The mixed liquor that adopts short chain alcohol and water is during as diluent, and filter membrane is selected organic system filter membrane.
8. method according to claim 1, is characterized in that: step 2) intermediate ion chromatography employing DIONEXICS3000 type ion chromatograph, detector is electric conductivity detector.
9. method according to claim 8, is characterized in that: the condition of ion chromatography is: anion analysisPost IonPacAS17C, specification 4mm × 250mm; Guard column IonPacAG17C, specification 4mm × 50mm; LeacheateFor KOH solution, gradient elution, gradient condition: 0.0～13.0min5mmol/L, 13.1～23.0min70mmol/L,23.1～30.0min5mmol/L, system flow rate is 0.8mL/min; Suppress electric current 174mA, sample size 25 μ L, when collectionBetween 30min.
10. method according to claim 1, is characterized in that: step 2) preparation method of Plays curve is:The standard substance of getting sweetener and anticorrisive agent is mixed with the mixed standard solution of series concentration, after ion chromatography with peak faceLong-pending tie substance concentration is done regression analysis, obtains the relation curve of material concentration and peak area.
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| CN107037174A (en) * | 2016-11-29 | 2017-08-11 | 赵会宇 | The assay method of the residual quantity of acesulfame potassium in hawthorn |
| CN107365627A (en) * | 2017-06-09 | 2017-11-21 | 广东中烟工业有限责任公司 | A kind of additive for being used to extend the tobacco aromaticss shelf-life |
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| CN108872448A (en) * | 2018-09-18 | 2018-11-23 | 国家烟草质量监督检验中心 | A kind of method that ultra performance liquid chromatography-tandem mass spectrum detects 5 kinds of sweeteners in flavouring essence for tobacco |
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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 |
| CN107037174A (en) * | 2016-11-29 | 2017-08-11 | 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 |
| CN107365627A (en) * | 2017-06-09 | 2017-11-21 | 广东中烟工业有限责任公司 | A kind of additive for being used to extend the tobacco aromaticss shelf-life |
| 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 |
| CN107367558A (en) * | 2017-07-06 | 2017-11-21 | 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 |
| 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 |
| CN108776187A (en) * | 2018-09-18 | 2018-11-09 | 国家烟草质量监督检验中心 | A kind of method that ultra performance liquid chromatography-tandem mass spectrum detects 5 kinds of sweeteners in cigarette tipping paper |
| CN108872448A (en) * | 2018-09-18 | 2018-11-23 | 国家烟草质量监督检验中心 | A kind of method that ultra performance liquid chromatography-tandem mass spectrum detects 5 kinds of sweeteners in flavouring essence for tobacco |
| CN108956840A (en) * | 2018-09-18 | 2018-12-07 | 国家烟草质量监督检验中心 | A kind of method that ultra performance liquid chromatography-tandem mass spectrum detects 5 kinds of sweeteners in electronic cigarette liquid |
| CN110763797A (en) * | 2019-11-12 | 2020-02-07 | 河南中烟工业有限责任公司 | Method for measuring sweetening agent for cigarettes by high performance liquid chromatography |
| 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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