CN106596805B - A kind of method of synthetic dyestuff in detection beverage based on DES liquid-liquid micro-extraction technologies - Google Patents
A kind of method of synthetic dyestuff in detection beverage based on DES liquid-liquid micro-extraction technologies Download PDFInfo
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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
Abstract
The present invention relates to a kind of method of synthetic dyestuff in detection beverage based on DES liquid-liquid micro-extraction technologies, belong to technical field of food detection.The present invention is prepared for a kind of new low temperature fused matter(The aliphatic acid of 8~10 carbon atoms and quaternary ammonium salt are synthetically prepared), as the extractant of liquid-liquid micro-extraction, it is applied to the method that 8 kinds of micro synthetic food colors in a kind of fast enriching, separation beverage in the enrichment analysis of 8 kinds of micro pigments, are established in beverage.
Description
Technical field
The present invention relates to a kind of method of synthetic dyestuff in detection beverage based on DES liquid-liquid micro-extraction technologies, belong to food
Product detection technique field.
Background technology
Food colour is most interested food additives.The color of food usually determines its attraction to consumer
Power.It is easy to due to the unstable of natural pigment and in process degrade,
So that synthetic food color is widely used [1].Edible synthetic coloring matter abbreviation synthetic dyestuff, to promote
The appetite of people, the non-nutritive composition for keeping food color bright-coloured and adding.Because synthetic dyestuff has bright in colour, tinting strength, tinting power
By force, be easy to that toning, property is stable and the advantages such as cost is cheap and be used widely [2].But exceeded, over range etc. is lack of standardization
Using the edible synthesized coloring matter that can then cause the passive excess intake of human body, cause belch, antimigraine, a variety of allergic symptoms occur
And the symptom [3] such as poisoning, What is more causes carcinogenic, teratogenesis, mutagenesis etc. to endanger [4].This is also to control in food
The main reason for synthetic dyestuff dosage.Therefore, establish method that is many while analyzing synthetic dyestuff in food.Including efficient liquid
Phase chromatography [5,6,7], AAS [8], thin-layered chromatography [9] etc..
Liquid-phase micro-extraction (LLME) since the advent of the world, due to it is simple to operate, extraction time is short, enrichment times are high, point
Analysis low cost and other advantages obtain great development.Big molten containing halogen of traditional liquid-liquid micro-extraction generally use density ratio water
Agent is extractant, but solvent containing halogen is because its toxicity is huge and readily volatilized, to environment and test operator
Health is a potential threat.Therefore, find a kind of requirement that can meet in traditional LLME to extractant, and can maximum journey
Extractant volatility and toxicity are reduced on degree, its " green extractant " to operating personnel's harm is reduced, by analytical chemistry work
Author more and more pays close attention to.
Low temperature fused matter (DES) was developed rapidly in recent years as a kind of new " green solvent ".It is by quaternary amine
Salt (Choline Chloride) is mixed with hydrogen bond donor (urea, glycerine, sugar, carboxylic acid etc.) with certain mol proportion, is interpenetrated in melting point,
Liquid mixture DES ([10,11,12] is formed during room temperature.Low temperature fused matter has biological degradability, without flammable, cheap, easy
The features such as preparing, be environment-friendly ([13,14,15,16].Therefore, various types of low temperature fused matters are produced, and are obtained wide
General application, just include as green solvent extracting isolating target compound [17] from various samples among these.Such as safflower
Middle phenolic metabolism thing extraction separation [18], Flavonoids from Plants extract [19], and heavy metal element extracts in biological sample
Analysis [20] etc. yields good result.These low temperature fused matters prepared are water solubility, are limited to a certain extent
Its application in aqueous specimen.
[1]Marta Kucharskaa,*,Jan Grabka.A review of chromatographic methods
for determination of synthetic food dyes[J].Talanta,2010,80:1045–1051.
[2] Kus E, Eroglu H E.Genotoxic and cytotoxic effects of sunset yellow
And brilliant blue, colorant food additives, on human blood lymphocytes [J]
.Pakistan journal of pharmaceutical sciences, 2015,28 (1):227-230.
[3]Goodman D W.Artificial food colour exclusion and free fatty acid
supplementation may reduce symptom severity in children with ADHD[J].Evidence
Based Mental Health, 2013,16 (3):77-77.
[4] Sarlkaya R, Selvi M,F.Evaluation ofpotential genotoxicity of
five food dyes using the somatic mutation and recombination test[J]
.Chemosphere, 2012,88 (8):974-979.
[5]Hao Wu,Jing-bo Guo,Li-ming Du.A rapid shaking-based ionic liquid
dispersive liquid phase microextraction for the simultaneous determination of
six synthetic food colourants in soft drinks,sugar-and gelatin-based
confectionery by high-performance liquid chromatography.Food Chemistry 141
(2013)182–186;
[6]Ou Sha,Xiashi Zhu,Yanli Feng,Weixing Ma.Aqueous two-phase based on
ionic liquid liquid–liquid microextraction for simultaneous determination of
ive synthetic food colourants in different food samples by high-performance
liquid chromatography.Food Chemistry 174(2015)380–386;
[7]Z.Zhang,L.Wang,X.Liu,D.Zhang,L.Zhang and Q.Li,RSC Adv.,2015.
[8]Turak&Ozgur,2013.
[9]Morlock&Oellig,2009.
[10]A.P.Abbott,G.Capper,D.L.Davies,R.K.Rasheed,V.Tambyrajah,
Chem.Commun.7(2003)70.
[11]A.P.Abbott,G.Capper,D.L.Davies,R.K.Rasheed,Inorg.Chem.43(2004)
3447.
[12]A.P.Abbott,D.Boothby,G.Capper,D.L.Davies,R.K.Rasheed,
V.Tambyrajah,J.Am.Chem.Soc.126(2004)9142.
[13]Y.Yu,X.Lu,Q.Zhou,K.Dong,H.Yao,S.Zhang,Chem.:Eur.J.14(2008)11174.
[14]K.D.Weaver,H.J.Kim,J.Sun,D.R.MacFarlane,G.D.Elliott,Green Chem.12
(2010)507.
[15]F.Ilgen,D.Ott,D.Kralish,C.Reil,A.Palmberger,B.Green Chem.11
(2009)1948.
[16]D.Reinhardt,F.Ilgen,D.Kralisch,B.G.Kreisel,Green Chem.10
(2008)1170.
[17]Baokun Tang,Heng Zhang,Kyung Ho Row,Application of deep eutectic
solvents in the extraction and separation of target compounds from various
samples,J.Sep.Sci.2015,38,1053–1064.
[18]Yuntao Dai,Geert-Jan Witkamp,Robert Verpoorte,and Young Hae Choi,
Natural Deep Eutectic Solvents as a New Extraction Media for Phenolic
Metabolites in Carthamus tinctorius L.Anal.Chem.2013,85,6272-6278.
[19]Wentao Bia,c,Minglei Tianb,c,Kyung Ho Row.Evaluation of alcohol-
based deep eutectic solvent in extraction and determination of lavonoids with
response surface methodology optimization,Journal of Chromatography A,1285
(2013)22–30.
[20]Kamal Ghanemi,Mohammad-Amin Navidi,Mehdi Fallah-Mehrjardi and Ali
Dadolahi-Sohrab, Ultra-fast microwave-assisted digestion in choline chloride-
oxalic acid deep eutectic solvent for determining Cu,Fe,Ni and Zn in marine
biological Samples,Anal.Met hods,2014,6,1774-1781.
The content of the invention
The invention provides a kind of new low temperature fused matter (tetrabutylammonium chloride:Octanoic acid).As liquid-liquid micro-extraction
Extractant, be applied in beverage in the enrichment analysis of 8 kinds of micro pigments, establish 8 in a kind of fast enriching, separation beverage
The method of the micro synthetic food color of kind.
Technical scheme is:
One side:
A kind of preparation method of low temperature fused matter, comprises the following steps:
Aliphatic acid containing 8~10 carbon atoms is well mixed with quaternary ammonium salt, after temperature reaction, that is, it is co-melting to obtain low temperature
Thing.
The described aliphatic acid containing 8~10 carbon atoms is selected from capric acid or octanoic acid.
Quaternary ammonium salt is selected from tri-n-octyl methyl ammonium chloride, tri-n-octyl methyl ammonium chloride, tetrabutylammonium chloride or tetrabutyl chlorine
Change ammonium.
The mol ratio of aliphatic acid and quaternary ammonium salt is 1:1~2, more preferably 1:1.2.
The temperature of temperature reaction is 35~45 DEG C, more preferably 40 DEG C;Reaction time is 15h, and becomes reaction solution
Bright supernatant liquid.
Second aspect:
The low temperature fused matter being directly prepared by the above method.
3rd aspect:
The method of synthetic dyestuff, comprises the following steps in a kind of detection beverage:
1st step, above-mentioned low temperature fused matter is added in drink sample, adds NaCl, and adjusted between pH to 3~9;
2nd step, extraction of ocean eddies, then low temperature fused matter is gone out by centrifugation, obtained low temperature fused matter is diluted in
In methanol, detected using liquid chromatography.
In the 1st described step, addition of the low temperature fused matter in drink sample is volume ratio 0.5~2:100, more preferably
It is 1:100.
In the 1st described step, it is also necessary to 3~8%NaCl of drink sample weight is added in drink sample, more preferably
5%.
In the 1st described step, the concentration range of the synthetic dyestuff in drink sample is 12g/mL, the choosing of described synthetic dyestuff
One or several kinds from lemon yellow, amaranth, sunset yellow, indigo, carmine, the red, light blue of temptation or erythrosine;It is described
Beverage be soda, tea beverage or fruit drink.
In the 2nd described step, the time of extraction of ocean eddies is 1~10min, more preferably 3min.
Beneficial effect
The present invention is prepared for a kind of new low temperature fused matter (tetrabutylammonium chloride:Octanoic acid).As liquid-liquid micro-extraction
Extractant, be applied in beverage in the enrichment analysis of 8 kinds of micro pigments, establish 8 in a kind of fast enriching, separation beverage
The method of the micro synthetic food color of kind.
Brief description of the drawings
Fig. 1 is influence block diagram of the different DES dosages to testing result;
Fig. 2 is influence block diagram of the different pH value to testing result;
Fig. 3 is influence block diagram of the different salt adding amounts to testing result;
Fig. 4 is influence block diagram of the different vortex times to testing result;
Embodiment
The present invention is described in further detail below by embodiment.But those skilled in the art will manage
Solution, the following example is merely to illustrate the present invention, and should not be taken as limiting the scope of the invention.Unreceipted specific skill in embodiment
Art or condition person, carried out according to the technology described by document in the art or condition or according to product description.Examination used
Agent or the unreceipted production firm person of instrument, being can be by the conventional products of acquisition purchased in market.Approximate language used herein is whole
It can be used for modifying any quantity statement in individual specification and claims, it can not cause its related basic function to occur
Permit being changed under conditions of change.Therefore, the value modified by term such as " about " is not limited to specified accurate
Value.In at least some cases, approximate language can be corresponding with the precision of the instrument for measuring the value.Unless context or sentence
In indicate otherwise, otherwise range limit can be combined and/or exchange, and this scope be confirmed as and including herein
Included all subranges.In addition to being indicated in embodiment is operated or elsewhere, specification and claims
Used in the amounts of all expression compositions, the numeral of reaction condition etc. or expression shall be construed as in all cases by
To the modification of word " about ".Word " comprising " used herein, "comprising", " having " or its any other variant are intended to cover non-
It is exclusive including.Technique, method, article or the equipment for e.g., including listing key element are not necessarily limited by those key elements, but can
So that this technique, method, article or the intrinsic key element of equipment are not expressly set out or belonged to including other.Expressed with range format
Value should be interpreted as not only including the numerical value as range limit that clearly includes in a flexible way, but also including culvert
All single numbers within the range or subinterval are covered, just as each numerical value and subinterval are expressly recited out.It is for example, " big
About 0.1% to about 5% " concentration range should be understood to not only include the concentration of about 0.1% to about 5% clearly included,
Also include allude in the range of single concentration (e.g., 1%, 2%, 3% and 4%) and subinterval (for example, 0.1% to 0.5%,
1% to 2.2%, 3.3% to 4.4%).
Instrument and reagent employed in following examples:
Laboratory apparatus
High performance liquid chromatograph (Shimadzu 20A);Temperature control magnetic stirring apparatus (German IKA companies);Vortex instrument (the morals of Genius 3
IKA companies of state);Glass syringe (25ml);
Reagent
Capric acid, octanoic acid, octadecanoid acid, tri-n-octyl methyl ammonium chloride, tetrabutylammonium chloride, DTAC
Purchased from into prompt chemical (Shanghai), lemon yellow, sunset yellow, indigo, carmine, the red, light blue of temptation and erythrosine standard items are purchased from north
Jing Zhen Xiangs company, purity > 98%.Methanol is chromatographically pure (Fisher companies of the U.S.), and other reagents are pure to analyze.Deionized water
Prepared by GenPure UV-TOC/UF × CAD plus (Thermo companies of the U.S.) Superpure water machine.
The chromatogram detection parameters of DES test liquids:
Standard liquid is prepared
1.0mL lemon yellows, amaranth are drawn respectively, sunset yellow, indigo, carmine, temptation is red, light blue, the mark of erythrosine
Quasi- product, by the use of deionized water constant volume as storing solution, save backup into 1000mL volumetric flasks in 4 DEG C of refrigerators.Before use, spend
Ionized water dilutes above-mentioned standard stock solution, is configured to the standard working solution of various concentrations, is preserved under the conditions of 4 DEG C.It is different dense
The mixed standard solution of degree is now with the current.
Chromatographic condition
Chromatographic column:C18 chromatographic columns (250mm × 4.6mm, 5mm);Column temperature:35℃;Sample size:10μL;Mobile phase:Flowing
Phase A is 0.02mol/L ammonium acetate solutions, and Mobile phase B is methanol, flow velocity 1mL/min;Gradient elution program:20%B exists
35%B is increased linearly in 5min, 98%B is then increased linearly in 7min, keeps 6min, it is finally linear in 0.1min
20%B is decremented to, keeps 8min.
It is prepared by embodiment 1DES
Prepare DES.Mol ratio weighs capric acid and quaternary ammonium salt and mixed into 50mL flasks respectively as shown in table 1, in 40 DEG C of oil
Heated in bath, until two mixtures become transparent supernatant liquid completely.It is standby after cooling to room temperature.
It is prepared by 1 different types of DES of table
The DES of embodiment 2 screening
Accurate commercially available certain the apple juice sample 10mL for drawing mark-on (adds lemon yellow, three-coloured amaranth in testing sample solution
Red, indigo, carmine, sunset yellow, red, erythrosine the concentration of temptation are all respectively 250ng/mL, and the concentration of light blue is 1 μ g/mL)
In 25mL glass syringes, example weight 5%NaCl is firstly added, 50 μ LDES is added and (is respectively adopted in embodiment 1 and makes
Standby 4 kinds of obtained DES), it is 6, extraction of ocean eddies 3min with HCl or NaOH regulations pH, DES is utilized to the injection ram of syringe
Be pushed into syringe port, the DES for drawing adsorpting pigment with micro-sampling pin in 2mL gland centrifuge tubes, repeat the above steps to
DES is suctioned out completely.1mL is settled to methanol dilution, is analyzed with sample introduction after 0.45 μm of membrane filtration.
With the four kinds of DES prepared extract respectively in mark-on drink sample 8 in synthetic dyestuff.No. 1 DES to it is carmine,
Red, erythrosine is lured without absorption, to synthetic dyestuff in 8 without absorption, No. 3 and No. 4 DES have No. 2 DES to synthetic dyestuff in 8
Absorption, No. 4 DES adsorption effects are more preferable.Therefore No. 4 DES (tetrabutylammonium chlorides are selected:Octanoic acid) it is the DES that this is tested.
The screening of the DES of embodiment 3 dosage
Accurate commercially available certain the apple juice sample 10mL for drawing mark-on (adds lemon yellow, three-coloured amaranth in testing sample solution
Red, indigo, carmine, sunset yellow, red, erythrosine the concentration of temptation are all respectively 250ng/mL, and the concentration of light blue is 1 μ g/mL)
In 25mL glass syringes, example weight 5%NaCl is firstly added, (dosage is respectively add in embodiment 1 No. 4 DES
20th, 50,80,100,150,200 μ L), it is 6, extraction of ocean eddies 3min with HCl or NaOH regulations pH, DES is utilized into syringe
Injection ram is pushed into syringe port, the DES of adsorpting pigment is drawn in 2mL gland centrifuge tubes with micro-sampling pin, in repetition
Step is stated to suction out completely to DES.1mL is settled to methanol dilution, is analyzed with sample introduction after 0.45 μm of membrane filtration.Each sample weight
It is multiple 5 times.
As shown in Figure 1:DES shows as competitive Adsorption when adsorbing hybrid pigment:Sunset yellow, famille rose, amaranth>Light blue
>Lemon yellow>Erythrosine, temptation are red>It is indigo, it is as a result as shown in the table.The dosage for considering final choice DES is 100 μ L.
Table 2
The screening of 3 solution ph to be measured of embodiment
Because the pH value of different beverages (soda, tea beverage, fruit drink etc.) has differences, it is contemplated that actual to answer
With being optimized the pH value of solution to be measured as a key factor.
Accurate commercially available certain the apple juice sample 10mL for drawing mark-on (adds lemon yellow, three-coloured amaranth in testing sample solution
Red, indigo, carmine, sunset yellow, red, erythrosine the concentration of temptation are all respectively 250ng/mL, and the concentration of light blue is 1 μ g/mL)
In 25mL glass syringes, example weight 5%NaCl is firstly added, add in embodiment 1 No. 4 DES100 μ L), use
HCl or NaOH adjusts pH respectively (3,4,5,6,7,8,9), extraction of ocean eddies 3min, and DES is utilized to the injection ram of syringe
Be pushed into syringe port, the DES for drawing adsorpting pigment with micro-sampling pin in 2mL gland centrifuge tubes, repeat the above steps to
DES is suctioned out completely.1mL is settled to methanol dilution, is analyzed with sample introduction after 0.45 μm of membrane filtration.Each sample is repeated 5 times.
As a result it is as shown in Figure 2.Lemon yellow, amaranth, famille rose, sunset yellow, light blue at pH value 3,6 adsorption effect compared with
Good, the indigo adsorption effect at pH value 5,6 is preferable, and the red adsorption effect at pH value 3,4,6 of temptation is preferable, and erythrosine is in pH value 6
Adsorption effect is preferable when~9, considers selection 6 and is used as optimum extraction pH value.
Table 3
The screening of the salt adding amount of embodiment 3
Because the pH value of different beverages (soda, tea beverage, fruit drink etc.) has differences, it is contemplated that actual to answer
With being optimized the pH value of solution to be measured as a key factor.
Accurate commercially available certain the apple juice sample 10mL for drawing mark-on (adds lemon yellow, three-coloured amaranth in testing sample solution
Red, indigo, carmine, sunset yellow, red, erythrosine the concentration of temptation are all respectively 250ng/mL, and the concentration of light blue is 1 μ g/mL)
In 25mL glass syringes, the NaCl of example weight 0~8% is firstly added, add in embodiment 1 No. 4 DES100 μ
L), it is respectively 6 to adjust pH with HCl or NaOH, extraction of ocean eddies 3min, DES is pushed into inject using the injection ram of syringe
Device mouth, the DES for drawing adsorpting pigment with micro-sampling pin repeat the above steps and inhaled completely to DES in 2mL gland centrifuge tubes
Go out.1mL is settled to methanol dilution, is analyzed with sample introduction after 0.45 μm of membrane filtration.Each sample is repeated 5 times.
For different salt adding amounts, the extraction efficiency of different pigments changes significantly, as shown in Figure 3.When adding for NaCl
When dosage is 4%, the extraction efficiency of various pigments is relatively satisfactory.
Table 4
The screening of the vortex time of embodiment 4
Accurate commercially available certain the apple juice sample 10mL for drawing mark-on (adds lemon yellow, three-coloured amaranth in testing sample solution
Red, indigo, carmine, sunset yellow, red, erythrosine the concentration of temptation are all respectively 250ng/mL, and the concentration of light blue is 1 μ g/mL)
In 25mL glass syringes, the NaCl of example weight 0~8% is firstly added, add in embodiment 1 No. 4 DES100 μ
L), it is respectively 6 to adjust pH with HCl or NaOH, the time that extraction of ocean eddies 10s~6min is not waited, and DES is utilized to the note of syringe
Penetrate piston and be pushed into syringe port, the DES for drawing adsorpting pigment with micro-sampling pin is repeated above-mentioned in 2mL gland centrifuge tubes
Step suctions out completely to DES.1mL is settled to methanol dilution, is analyzed with sample introduction after 0.45 μm of membrane filtration.Each sample repeats
5 times.
The raising of vortex time contributes to partition equilibrium of the object between DES and the aqueous solution, while promotes the rate of recovery
Raising.Influence of the vortex time to extraction efficiency of this experiment investigation, as a result as shown in Figure 4.In 1 to 3min, with extraction
Taking the growth extraction efficiency of time also gradually increases, and reaches maximum when the time is 3min, be during 5min the longer time again
Without significant change.
Table 5
The methodological study of embodiment 5
Under optimal experiment condition, a kind of analysis method of various pigments in new quantitative analysis beverage is established.For
The performance of evaluation institute method for building up, respectively to working curve, the range of linearity, coefficient correlation, detection limit and quantitative limit and again
Renaturation is investigated.Selection mark-on sample carries out analysis measure.The reappearance day to day precision of this extracting process and in a few days
Precision data is assessed.
1. the range of linearity and quantitative limit
The serial hybrid standard working solution of 8 kinds of object various concentrations is prepared respectively, with target components peak area to corresponding
Concentration carries out linear regression, corresponding during using the signal to noise ratio of testing compound chromatographic peak in mark-on sample as 3 times of noise signal
Measured object concentration value calculate detection limit (LODs), the results are shown in Table 6.
The linear of 68 kinds of pigment detection methods of table, precision, detection limit
2. the rate of recovery and precision of method
It is molten that different amounts of hybrid standard is added in 3 kinds of different beverage (soda, tea beverage, fruit drink) matrix
Liquid, it is respectively 1.0,10.0,50.0 μ g/kg that the mark-on of 8 kinds of pigments is horizontal, each level set 5 it is parallel.By above-mentioned optimal bar
Part is handled and determined, and is calculated the rate of recovery and relative standard deviation of relative target thing, be the results are shown in Table 7.
The rate of recovery and relative standard deviation (n=5) of 8 kinds of target compounds in the beverage of table 7
Claims (1)
- A kind of 1. method for detecting synthetic dyestuff in beverage, it is characterised in that comprise the following steps:1st step, in drink sample Low temperature fused matter is added, adds NaCl, and is adjusted between pH to 3~9;2nd step, extraction of ocean eddies, then low temperature fused matter is passed through Cross and centrifuge out, by the dilution of obtained low temperature fused matter in methyl alcohol, detected using liquid chromatography;The preparation method of low temperature fused matter described in 1st step comprises the following steps:Aliphatic acid containing 8~10 carbon atoms is well mixed with quaternary ammonium salt, after temperature reaction, that is, obtains low temperature fused matter;The described aliphatic acid containing 8~10 carbon atoms is octanoic acid;Quaternary ammonium salt is tetrabutylammonium chloride;The mol ratio of aliphatic acid and quaternary ammonium salt is 1:1.2;The temperature of temperature reaction is 40 DEG C;Reaction time is 15h, and reaction solution is become transparent supernatant liquid;In the 1st described step, addition of the low temperature fused matter in drink sample is volume ratio 1:100;In the 1st described step, Also need to add the 5%NaCl of drink sample weight in drink sample;In the 1st described step, the concentration range of the synthetic dyestuff in drink sample is 12g/mL, and described synthetic dyestuff is selected from One or several kinds in lemon yellow, amaranth, sunset yellow, indigo, carmine, the red, light blue of temptation or erythrosine;Described Beverage is soda, tea beverage or fruit drink;In the 2nd described step, the time of extraction of ocean eddies is 3min;C18 posts are used in liquid chromatography;Mobile phase includes:Mobile phase A is 0.02 mol/L ammonium acetate solutions, flowing Phase B is methanol, and flow velocity is 1 mL/ min;Gradient elution program is:First by the percent by volume of Mobile phase B in 5 min It is interior to increase linearly to 35 % from 20 %, 98% Mobile phase B is then increased linearly in 7min again, 6 min is kept, finally exists 20% Mobile phase B is linearly decremented in 0.1min, keeps 8min.
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