CN106596805A - Method for detecting synthetic pigments in beverage based on DES liquid-liquid microextraction technology - Google Patents
Method for detecting synthetic pigments in beverage based on DES liquid-liquid microextraction technology Download PDFInfo
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Abstract
The invention relates to a method for detecting synthetic pigments in a beverage based on DES liquid-liquid microextraction technology, and belongs to the technical field of food inspection. A new low temperature eutectic substance (prepared from a fatty acid with 8-10 carbon atoms and a quaternary ammonium salt) is used as an extraction solvent for liquid-liquid microextraction, and is used in enrichment and analysis of 8 trace pigments in the beverage, and a method for rapid enrichment and separation of the 8 trace synthetical pigments in the beverage is established.
Description
Technical field
The present invention relates to a kind of method for detecting synthetic dyestuff in beverage based on DES liquid-liquid micro-extraction technologies, belongs 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 degraded due to the unstable of natural colouring matter and in process,
So that synthetic food color is widely used [1].Edible synthetic coloring matter abbreviation synthetic dyestuff, is enhancement
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, it is easy to the advantage such as toning, stable in properties and with low cost and is 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, various allergic symptoms occur
And poisoning etc. symptom [3], What is more causes carcinogenic, teratogenesis, mutagenesis etc. endanger [4].This is also must to control in food
The main cause of synthetic dyestuff consumption.For this purpose, establishing many methods for analyzing synthetic dyestuff in food simultaneously.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 simple to operate, extraction time it is short, enrichment times are high, point
Analysis low cost and other advantages obtain greatly development.Traditional liquid-liquid micro-extraction is generally using big molten containing halogen of density ratio water
Agent is extractant, but solvent containing halogen is huge and readily volatilized due to its toxicity, to environment and test operation personnel
Health is a potential threat.For this purpose, find a class can meet to the requirement of extractant in traditional LLME, 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, easily
The features such as preparation, environmental friendliness ([13,14,15,16].Therefore, various types of low temperature fused matters are produced, and obtain wide
General application, just includes isolating target compound [17] is extracted from various samples as green solvent among these.Such as safflower
Middle phenolic metabolism thing is extracted and separates [18], and Flavonoids from Plants extracts [19], and heavy metal element is extracted in biological sample
Analysis [20] etc. is yielded good result.These low temperature fused matters for preparing are water solubility, limit 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, in being applied in beverage the enrichment analysis of 8 kinds of micro pigments, establish a kind of fast enriching, separate 8 in beverage
The method for planting micro synthetic food color.
Technical scheme is：
One side：
A kind of preparation method of low temperature fused matter, comprises the steps：
Aliphatic acid containing 8～10 carbon atoms is well mixed with quaternary ammonium salt, after temperature reaction, that is, low temperature is obtained co-melting
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.
Aliphatic acid is 1 with the mol ratio of quaternary ammonium salt：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 reactant liquor
Bright supernatant liquid.
Second aspect：
The low temperature fused matter directly prepared by said method.
3rd aspect：
The method of synthetic dyestuff, comprises the steps in a kind of detection beverage：
1st step, adds above-mentioned low temperature fused matter in drink sample, adds NaCl, and adjusts between pH to 3～9；
2nd step, extraction of ocean eddies, then low temperature fused matter is gone out through centrifugation, the low temperature fused matter for obtaining is diluted in
In methyl alcohol, 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, in addition 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, described synthetic dyestuff choosing
From lemon yellow, amaranth, sunset yellow, it is indigo, carmine, lure in red, light blue or erythrosine one or several；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, in being applied in beverage the enrichment analysis of 8 kinds of micro pigments, establish a kind of fast enriching, separate 8 in beverage
The method for planting micro synthetic food color.
Description of the drawings
Fig. 1 is impact block diagram of the different DES consumptions to testing result；
Fig. 2 is impact block diagram of the different pH value to testing result；
Fig. 3 is impact block diagram of the different salt adding amounts to testing result；
Fig. 4 is impact block diagram of the different vortex times to testing result；
Specific embodiment
The present invention is described in further detail below by specific 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 concrete skill in embodiment
Art or condition person, are carried out according to the technology or condition described by document in the art or according to product description.Examination used
Agent or the unreceipted production firm person of instrument, be can pass through city available from conventional products.Approximate language used herein is whole
Can be used to modify any quantity statement in individual specification and claims, it can occur in the basic function for not causing its related
Permit being changed under conditions of change.Therefore, it is accurate specified by the value of term modification such as " about " is not limited to
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 is confirmed as and including herein
Included all subranges.Except operation embodiment in or elsewhere in indicate in addition to, specification and claims
Used in amount, the reaction condition of all expression compositions etc. numeral or expression shall be construed as receiving in all cases
To the modification of word " about ".Word " including " used herein, "comprising", " having " or its any other variant are intended to cover non-
It is exclusive including.For example, those key elements are not necessarily limited by including technique, method, article or the equipment for listing key element, but can
The key element intrinsic so that this technique, method, article or equipment are not expressly set out or belonged to including other.With range format expression
Value should be interpreted as in a flexible way not only including the numerical value as range limit that clearly includes, 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.For example, it is " big
About 0.1% to about 5% " concentration range should be understood to the concentration of about 0.1% to about 5% for not only including clearly including,
Also include single concentration in the range of alluding to (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 chemistry (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%.Methyl alcohol is chromatographically pure (Fisher companies of the U.S.), and other reagents are pure for analysis.Deionized water
Prepared by GenPure UV-TOC/UF × CAD plus (Thermo companies of the U.S.) Superpure water machine.
The chromatogram detection parameter of DES test liquids：
Standard liquid is prepared
1.0mL lemon yellows, amaranth, sunset yellow, indigo, carmine, the red, light blue of temptation, the mark of erythrosine are drawn respectively
Into 1000mL volumetric flasks, deionized water constant volume is saved backup quasi- product as storing solution in 4 DEG C of refrigerators.Using front, spend
Ionized water dilutes above-mentioned standard stock solution, is configured to the standard working solution of variable concentrations, preserves 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 methyl alcohol, and flow velocity is 1mL/min；Gradient elution program：20%B exists
35%B is increased linearly in 5min, 98%B is then increased linearly in 7min, keep 6min, it is finally linear in 0.1min
20%B is decremented to, 8min is kept.
It is prepared by embodiment 1DES
Prepare DES.The mol ratio as shown in table 1 weighs respectively capric acid and quaternary ammonium salt and mixes into 50mL flasks, in 40 DEG C of oil
Heat in bath, until two mixtures become completely transparent supernatant liquid.Cool to room temperature standby.
It is prepared by the different types of DES of table 1
The screening of the DES of embodiment 2
Accurately draw plus commercially available certain apple juice sample 10mL of target (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, adds 50 μ LDES and (be respectively adopted in embodiment 1 and make
The standby 4 kinds of DES for obtaining), it is 6, extraction of ocean eddies 3min to adjust pH with HCl or NaOH, and DES is utilized into the injection ram of syringe
Syringe port is pushed into, the DES of adsorpting pigment is drawn in 2mL gland centrifuge tubes with micro-sampling pin, repeat the above steps are extremely
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 for preparing 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) be this experiment DES.
The screening of the consumption of the DES of embodiment 3
Accurately draw plus commercially available certain apple juice sample 10mL of target (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, (consumption is respectively to add in embodiment 1 No. 4 DES
20th, 50,80,100,150,200 μ L), it is 6, extraction of ocean eddies 3min to adjust pH with HCl or NaOH, by DES using syringe
Injection ram is pushed into syringe port, and the DES of adsorpting pigment is drawn in 2mL gland centrifuge tubes, in repetition with micro-sampling pin
State step 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 hybrid pigment is adsorbed：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 consumption for considering final choice DES is 100 μ L.
Table 2
The screening of the solution ph to be measured 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.
Accurately draw plus commercially available certain apple juice sample 10mL of target (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, adds No. 4 DES100 μ L in embodiment 1), use
HCl or NaOH adjusts pH and is respectively (3,4,5,6,7,8,9), extraction of ocean eddies 3min, and DES is utilized into the injection ram of syringe
Syringe port is pushed into, the DES of adsorpting pigment is drawn in 2mL gland centrifuge tubes with micro-sampling pin, repeat the above steps are extremely
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 preferably, lures the red adsorption effect at pH value 3,4,6 preferably, and erythrosine is in pH value 6
Adsorption effect preferably, considers selection 6 as optimum extraction pH value when～9.
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.
Accurately draw plus commercially available certain apple juice sample 10mL of target (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, adds No. 4 DES100 μ in embodiment 1
L), adjust pH with HCl or NaOH and be respectively 6, extraction of ocean eddies 3min, DES is pushed into into injection using the injection ram of syringe
Device mouth, the DES of adsorpting pigment is drawn in 2mL gland centrifuge tubes with micro-sampling pin, and repeat the above steps to DES inhales completely
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 is changed 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
Accurately draw plus commercially available certain apple juice sample 10mL of target (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, adds No. 4 DES100 μ in embodiment 1
L), adjust pH with HCl or NaOH and be respectively 6, the time that extraction of ocean eddies 10s～6min is not waited, DES is utilized into the note of syringe
Penetrate piston and be pushed into syringe port, the DES of adsorpting pigment is drawn in 2mL gland centrifuge tubes with micro-sampling pin, repetition is above-mentioned
Step 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 repeats
5 times.
The raising of vortex time contributes to partition equilibrium of the object between DES and the aqueous solution, while promoting the rate of recovery
Raising.Impact 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, when the time be 3min when reach maximum, 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 institute's method for building up is evaluated, respectively to working curve, the range of linearity, coefficient correlation, detection limit and quantitative limit and weight
Renaturation is investigated.Mark-on sample is selected to be analyzed measure.The reappearance day to day precision of this extracting process and in a few days
Precision data is assessing.
1. the range of linearity and quantitative limit
The serial hybrid standard working solution of 8 kinds of object variable concentrations is prepared respectively, with target components peak area to corresponding
Concentration carries out linear regression, and the signal to noise ratio with testing compound chromatographic peak in mark-on sample is corresponding when being 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
Add different amounts of hybrid standard in 3 kinds of different beverage (soda, tea beverage, fruit drink) matrix molten
Liquid, the mark-on level of 8 kinds of pigments is respectively 1.0,10.0,50.0 μ g/kg, each level set 5 it is parallel.By above-mentioned optimum bar
Part is processed and determined, and calculates the rate of recovery and relative standard deviation of relative target thing, the results are shown in Table 7.
The rate of recovery of 8 kinds of target compounds and relative standard deviation (n=5) in the beverage of table 7
Claims (10)
1. a kind of preparation method of low temperature fused matter, it is characterised in that comprise the steps：By containing 8～10 carbon atoms
Aliphatic acid is well mixed with quaternary ammonium salt, after temperature reaction, that is, obtains low temperature fused matter.
2. the preparation method of low temperature fused matter according to claim 1, it is characterised in that described containing 8～10 carbon
The aliphatic acid of atom is selected from capric acid or octanoic acid, more preferably octanoic acid.
3. the preparation method of low temperature fused matter according to claim 1, it is characterised in that quaternary ammonium salt is selected from tricaprylmethyl
Ammonium chloride, tri-n-octyl methyl ammonium chloride, tetrabutylammonium chloride or tetrabutylammonium chloride, more preferably tetrabutylammonium chloride.
4. the preparation method of low temperature fused matter according to claim 1, it is characterised in that aliphatic acid and quaternary ammonium salt mole
Than being 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 make reactant liquor become transparent supernatant liquid.
5. the low temperature fused matter that the method described in claim 1 is obtained.
6. it is a kind of detection beverage in synthetic dyestuff method, it is characterised in that comprise the steps：1st step, in drink sample
The low temperature fused matter described in claim 5 is added, NaCl is added, and is adjusted between pH to 3～9；2nd step, extraction of ocean eddies, then
Low temperature fused matter is gone out through centrifugation, the low temperature fused matter for obtaining is diluted in methyl alcohol, carried out using liquid chromatography
Detection.
7. it is according to claim 6 detection beverage in synthetic dyestuff method, it is characterised in that it is low in the 1st described step
Addition of the warm fused matter in drink sample is volume ratio 0.5～2：100, more preferably 1：100；In the 1st described step, also
3～8%NaCl of needs addition drink sample weight in drink sample, more preferably 5%.
8. it is according to claim 6 detection beverage in synthetic dyestuff method, it is characterised in that 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 lemon yellow, amaranth, sunset
It is yellow, indigo, carmine, lure in red, light blue or erythrosine one or several；Described beverage is soda, tea
Beverage or fruit drink.
9. it is according to claim 6 detection beverage in synthetic dyestuff method, it is characterised in that in the 2nd described step, whirlpool
The time that rotation is extracted is 1～10min, more preferably 3min.
10. it is according to claim 6 detection beverage in synthetic dyestuff method, it is characterised in that adopt in liquid chromatography
Use C18 posts；Mobile phase is included：Mobile phase A is 0.02 mol/L ammonium acetate solutions, and Mobile phase B is methyl alcohol, and flow velocity is 1
mL/ min；Gradient elution program is：The percent by volume of Mobile phase B is increased linearly in 5 min from 20 % first
35 %, then increase linearly in 7min again 98% Mobile phase B, keep 6 min, are finally linearly decremented in 0.1min
20% Mobile phase B, keeps 8min.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN106990183A (en) * | 2017-05-05 | 2017-07-28 | 蚌埠市疾病预防控制中心 | The method for chromatographic determination of synthetic coloring matter in a kind of food |
| CN109115898A (en) * | 2018-06-14 | 2019-01-01 | 浙江工业大学 | Method for analyzing pesticide residues in water sample by using double-aqueous-phase system based on eutectic solvent-inorganic salt |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106990183A (en) * | 2017-05-05 | 2017-07-28 | 蚌埠市疾病预防控制中心 | The method for chromatographic determination of synthetic coloring matter in a kind of food |
| CN109115898A (en) * | 2018-06-14 | 2019-01-01 | 浙江工业大学 | Method for analyzing pesticide residues in water sample by using double-aqueous-phase system based on eutectic solvent-inorganic salt |
| CN109115898B (en) * | 2018-06-14 | 2021-07-27 | 浙江工业大学 | Method for analyzing pesticide residues in water sample by using double-aqueous-phase system based on eutectic solvent-inorganic salt |
| CN111679024A (en) * | 2020-07-21 | 2020-09-18 | 甘肃省食品检验研究院 | Preparation of hydrophobic low-temperature eutectic and method for extracting Congo red, acid golden yellow and red 2G in meat products and aquatic products |
Also Published As
| Publication number | Publication date |
|---|---|
| CN106596805B (en) | 2018-02-27 |
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