CN104849389B - The method of spice in a kind of ionic liquid aqueous two-phase extraction/HPLC detection rice - Google Patents
The method of spice in a kind of ionic liquid aqueous two-phase extraction/HPLC detection rice Download PDFInfo
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Abstract
The invention belongs to technical field of food safety detection, specifically disclose the method for spice in a kind of ionic liquid aqueous two-phase extraction/HPLC detection rice.The present invention first extracts with [Bmim] Cl/ dipotassium hydrogen phosphate double-aqueous phase system, then analyze in conjunction with HPLC, in [Bmim] Cl/ dipotassium hydrogen phosphate double-aqueous phase system used, the mass fraction of [Bmim] Cl is 10 ~ 25%, and the mass fraction of dipotassium hydrogen phosphate is 30 ~ 50%.The present invention has detecting step operation simple, easy, detection limits low, advantages of environment protection, has relatively broad application prospect in field of food detection.
Description
Technical field
The present invention relates to technical field of food safety detection, more particularly, to a kind of ionic liquid aqueous two-phase extraction/
The method of spice in HPLC detection rice.
Background technology
The population of China more than 2/3rds is with rice as staple food.Along with the raising of people's living standard, the food to rice
Having higher requirement by quality, scented rice receives the welcome of consumer.But also cannot meet in scented rice total amount at present and disappear
The person's of expense demand, has caused people to use rice essence in the rice production course of processing because interests are ordered about, to pretend to be scented rice.More have
Notably, adding rice essence in old rice pretends to be new rice to cheat consumer.Relevant document report rice essence main component or
Dispensing has propylene glycol, 2-acetylpyridine, vanillin, ethyl vanillin and ethylmaltol etc..Vanillin therein and ethyl
Maltol and respective homologue ethyl vanillin and maltol are broad spectrum type spice, are widely used in the preparation of essence, are rice
The fragrance component that essence is conventional in producing.But relevant research shows that these spice of Excess free enthalpy can cause dizziness, Nausea and vomiting
And dyspnea, even affect liver and renal function.When the staple food of rice of people with the addition of rice essence, can be the biggest
The big exposure level increasing people and these additives, the most in the past, can bring serious infringement, especially child to health
And teenager, they also do not grow also in trophophase, various functions organ completely.GB 2760-2011 " food safety simultaneously
National standard food additive uses standard " in define in 27 kinds of food such as rice and must not add essence and flavoring agent.Therefore detect
Spice in rice has very important significance to ensuring food safety.
It is currently used for detecting the method for spice in food and mainly has spectrophotography, HPLC, GC, LC/MS etc..HPLC method by
High in the accuracy of detection, sensitivity is good, many kinds of substance can be realized while detection and the advantage such as testing cost is low, it has also become fragrant
The main flow means of material detection.The pre-treating method reported mainly has the method such as solvent extraction, Solid-Phase Extraction.Solvent extraction method is adopted
Use a large amount of organic solvent, not only pollute the environment, and the impurity extracted is more, the accuracy of impact detection.Solid phase extracts
Although following the example of the interference that can reduce impurity, but use during the activation of pillar to be experienced, adsorbed target thing, eluting impurity, wash
The series of steps such as de-object, complex operation is time-consuming, is not suitable for the process of batch sample.Simultaneously because the solid phase extraction of commercialization
Take pillar price higher, the most also can be greatly increased testing cost.
Summary of the invention
The present invention is in order to overcome the above-mentioned deficiency of prior art, it is provided that a kind of ionic liquid aqueous two-phase extraction/HPLC detection
The method of spice in rice.The present invention uses ionic liquid double-aqueous phase system to extract the spice in rice, and uses HPLC method to enter
Row detection.Due to the feature of ionic liquid aqueous two-phase extraction be homogeneously extraction out-phase separate, therefore can realize extract, purify with
Step completes, and greatly reduces operating procedure, simultaneously because the amount of the ionic liquid used in this system and inorganic salt is less, therefore
Running cost is greatly reduced, and the detection that can meet batch sample processes.On the whole the method have simple to operate, extract clean
Change efficiency height, detect fireballing feature, it is possible to achieve quick, the efficient detection of spice in rice.
To achieve these goals, the present invention is achieved by below scheme:
The method of spice in a kind of ionic liquid aqueous two-phase extraction/HPLC detection rice, comprises the following steps:
S1. extraction: add [Bmim] Cl/ dipotassium hydrogen phosphate double-aqueous phase system in rice by the mass ratio of 1:5 ~ 20, mixed
20 ~ 50 DEG C of water-bath 10 ~ 40min after even, phase solution in taking-up；
Wherein, in [Bmim] Cl/ dipotassium hydrogen phosphate double-aqueous phase system, the mass fraction of [Bmim] Cl is 10 ~ 25%, phosphoric acid hydrogen
The mass fraction of dipotassium is 30 ~ 50%；
S2.HPLC detects: is diluted by upper phase solution with flowing phase solution, carries out HPLC analysis, paint after filtering with microporous membrane
Standard curve processed and recovery of standard addition.
Ionic liquid double-aqueous phase system is generally formed by a kind of organic salt, a kind of inorganic salt and water, and conventional organic salt is
[Bmim]Cl、[Hmim]Cl、[Omim]Cl、[Dmim]Cl、[Bmmim]Cl、[BPy]Cl、[TBA]Cl、[TBP]Cl、[Bmim]
Br、[TBA]Br、[Bmim]BF4、[BPy]BF4、[Bmim]NO3；Conventional inorganic salt is potassium phosphate, disodium hydrogen phosphate, phosphoric acid
Hydrogen dipotassium, sodium dihydrogen phosphate, ammonium sulfate, potassium carbonate, sodium carbonate, potassium hydroxide, sodium hydroxide；Different organic salt and inorganic salt
The performance of the double-aqueous phase system that collocation is formed is different.The present invention is according to spice especially maltol, ethylmaltol, chinese cymbidium
Element, the construction features of ethyl vanillin, develop [Bmim] Cl/ dipotassium hydrogen phosphate aqueous two-phase body of a kind of applicable extraction spice
System.
Preferably, in system, the mass fraction of [Bmim] Cl is 15%, and the mass fraction of dipotassium hydrogen phosphate is 35%.
Preferably, the mass ratio of rice and [Bmim] Cl/ dipotassium hydrogen phosphate double-aqueous phase system is 1:10.
Preferably, described in S2, HPLC detection is to use Atlantis C18Chromatographic column (150 mm × 4.6 mm, 5 μm),
Flowing is acetonitrile-0.5% formic acid solution mutually, and flow velocity is 1.0 mL/min, and detection wavelength is 276 nm, column temperature 30 DEG C, sample size 10
μL。
Preferably, with flowing phase solution, upper phase solution is diluted 2 ~ 5 times.
The drawing process of described standard curve is: takes blank rice sample, carries out pre-treatment according to step S1, obtain blank
Sample extracting solution.Using blank sample extracting solution as the diluent of spice standard substance, prepare a series of standard working solution:
0.5,1.0,2.0,5.0,10.0,25.0 μ g/mL, after above-mentioned standard working solution is crossed 0.22 μm membrane filtration, sample introduction divides
Analysis, each concentration parallel assay 2 ~ 4 times, qualitative with retention time, quantitative, with face, peak with peak area ratio with sample peak area
Concentration C (μ g/mL) is returned and obtains standard regression curve by long-pending A.
The determination step of described recovery of standard addition is: takes blank rice sample, adds a certain amount of spice hybrid standard molten
Liquid, makes spice content in rice be respectively 1.0,2.0,10.0 mg/kg, takes 0.2 g and add target sample after mixing, according to
The process of step S1.In on the same day, each spiked levels carries out 4 ~ 6 repetitions, METHOD FOR CONTINUOUS DETERMINATION 5 ~ 6 days, the recovery of assay method
Rate and withinday precision and day to day precision.
Compared with prior art, the method have the advantages that
Using ionic liquid aqueous two phase extraction technique as in rice spice detection sample-pretreating method, using HPLC as
Detection means, by optimizing chromatographic isolation parameter and extraction conditions such as flowing phase kind, type of elution, ionic liquid and inorganic salt
Kind and consumption, bath temperature, water bath time etc., set up a kind of extraction and cleaning synchronously complete, detection method easy and simple to handle.This
Invention has accurately and reliably, highly sensitive, advantages of environment protection, it is adaptable to the detection of spice in rice.
Accompanying drawing explanation
Fig. 1 is four kinds of spice standard substance chromatograms；1: maltol；2: ethylmaltol；3: vanillin；4: ethyl chinese cymbidium
Element.
Fig. 2 is blank rice sample chromatogram.
Fig. 3 is mark-on rice sample chromatogram；1: maltol；2: ethylmaltol；3: vanillin；4: ethyl vanillin.
Detailed description of the invention
Below in conjunction with Figure of description and specific embodiment the present invention made and elaborating further, described embodiment
It is served only for explaining the present invention, is not intended to limit the scope of the present invention.Test method used in following embodiment is as without special
Different explanation, is conventional method；The material that used, reagent etc., if no special instructions, for the reagent commercially obtained
And material.
Embodiment 1
The screening of ionic liquid double-aqueous phase system:
During preliminary experiment, do the ionic liquid double-aqueous phase system of following several types altogether: [Bmim] Cl/ sulphuric acid
Ammonium, [Bmim] Cl/ sodium sulfate, [Bmim] Cl/ sodium carbonate, [Bmim] Cl/ sodium chloride, [Bmim] Cl/ dipotassium hydrogen phosphate,
[Omim] Cl/ammonium sulfate, [Omim] Cl/sodium sulfate, [Omim] Cl/sodium carbonate, [Omim] Cl/sodium chloride, [Omim] Cl
/ dipotassium hydrogen phosphate, [Bmim] BF4/ ammonium sulfate, [Bmim] BF4/ sodium sulfate, [Bmim] BF4/ sodium carbonate, [Bmim] BF4 /
Sodium chloride, [Bmim] BF4/ dipotassium hydrogen phosphate, however, it was found that [Bmim] Cl/ dipotassium hydrogen phosphate aqueous two-phase of only consisting of
System: the mass fraction of [Bmim] Cl is 10 ~ 25%, the mass fraction of dipotassium hydrogen phosphate is 30 ~ 50%；It is suitable for the extraction of spice
Take.
Embodiment 2
The rice of the present embodiment is general rice, spice in a kind of ionic liquid aqueous two-phase extraction/HPLC detection rice
Method, it concretely comprises the following steps:
1, the preparation of four kinds of spice (maltol, ethylmaltol, vanillin, ethyl vanillin) standard reserving solutions: accurately
Weighing 0.0100 g(to be accurate to 0.0001 g) each standard substance sterling is in small beaker, with 15%(V/V) acetonitrile solution dissolves also
Be settled in 10 mL volumetric flasks, be placed in 4 DEG C of refrigerators are laid in stand-by.
2, sample pre-treatments: first preparation gross mass is the ionic liquid double-aqueous phase system of 2 g, this system intermediate ion liquid
The quality of ([Bmim]) is 0.3 g(15%, w/w), the quality of dipotassium hydrogen phosphate is 0.7g(35%, w/w) quality of water is 1.0 g
(50%, w/w).Add rice articles for use 0.2 g after system configurations is good, after rocking mixing, be placed on water-bath in the water-bath of 40 DEG C
15min.Take out upper phase solution, i.e. ionic liquid phase afterwards, with flowing phase solution (acetonitrile-0.5% formic acid solution) constant volume to 2
ML, then take part solution cross 0.22 the laggard HPLC of μm microporous filter membrane analyze.
3, chromatographic condition
Chromatographic column: Atlantis C18(150 mm × 4.6 mm, 5 μm)；Flowing phase: acetonitrile-0.5% formic acid solution；Ladder
Degree eluting: program is shown in Table 1；Flow velocity: 1 mL/min；Column temperature: 30 DEG C；Detection wavelength: 276 nm；Sample size: 10 μ L.
Table 1 gradient elution program
4, Specification Curve of Increasing
Take blank rice sample, carry out pre-treatment according to step 2, obtain blank sample extracting solution.Blank sample is extracted
Liquid, as the diluent of spice standard substance, prepares a series of standard working solution: 0.5,1.0,2.0,5.0,10.0,25.0 μ
G/mL, crosses sample introduction analysis after 0.22 μm membrane filtration by above-mentioned standard working solution, and each concentration parallel assay 3 times, during to retain
Between qualitative, quantitative with sample peak area and peak area ratio, with peak area A concentration C (μ g/mL) returned and obtains standard and return
Return curve.
5, recovery of standard addition
Take blank rice sample, add a certain amount of spice mixed standard solution, make spice content in rice respectively
It is 1.0,2.0,10.0 mg/kg, takes 0.2 g after mixing and add target sample, process according to step 2.Each add on the same day
Mark concentration carries out 5 times and repeats, METHOD FOR CONTINUOUS DETERMINATION 5 days, the response rate of assay method and withinday precision and day to day precision.
Below by experimental data, testing result is analyzed.
1, chromatogram
The ionic liquid that the present invention chooses is [Bmim] Cl, and becoming phase salt is dipotassium hydrogen phosphate, and both can be wider dense
Become phase in the range of degree, be conducive to fast rapid-result phase.When ionic liquid mass fraction in double-aqueous phase system is less than 15%, target
The response rate of thing is relatively low, meets and analyzes requirement.When ionic liquid mass fraction in double-aqueous phase system is more than 15%, along with
The increase of ionic liquid mass fraction, the response rate has the trend of increase, but is to increase inconspicuous, therefore selects in double-aqueous phase system
The mass fraction of ionic liquid is 15%.Fig. 1 to Fig. 3 is respectively the standard solution chromatogram of acetontrile, blank rice sample color
Spectrogram and rice mark-on sample chromatogram figure, when from figure, contrast is it can be seen that ionic liquid aqueous two-phase does pre-treating method, sample liquid
Impurity in middle extraction is little, and ionic liquid cognition went out peak, thus without affecting object before object is eluted
Measure.Wherein the retention time of maltol is: 3.79, and the retention time of ethylmaltol is 7.20, the retention time of vanillin
Being 8.08, the retention time of ethyl vanillin is 10.80.
2, the range of linearity of method, sample recovery of standard addition, withinday precision and day to day precision
The range of linearity of four kinds of spice and respective regression equation are shown in Table 2, and sample recovery of standard addition is shown in Table 3 and table 4 respectively.
The range of linearity of four kinds of materials is 1.0 ~ 50.0 μ g/mL as shown in Table 2, and linear relationship is good, and correlation coefficient is all higher than 0.999.
From table 3 and table 4, under different spiked levels, the recovery of standard addition of sample is between 95.34 ~ 104.85%, relative standard deviation
Between 2.47 ~ 4.71%.Method RSD in the daytime is less than 4.47%, and RSD is less than 4.79% in the daytime.
The range of linearity of 2 four kinds of spice of table, regression equation, correlation coefficient
Table 3 sample recovery of standard addition
Table 4 method in a few days with day to day precision
The present invention have studied a kind of ionic liquid aqueous two-phase extraction/HPLC and measures method and the chromatostrip of spice in rice
Part.[Bmim] Cl-dipotassium hydrogen phosphate ionic liquid double-aqueous phase system has good extraction ability to the spice in rice, in conjunction with
High performance liquid chromatography is as detection means, it is possible to achieve the detection accurately and rapidly of spice in rice.
The experiment condition obtained optimized is: [Bmim] Cl concentration 15%(w/w in system), dipotassium hydrogen phosphate concentration 35%
(w/w), bath temperature 40 DEG C, water bath time 15 min.Use Atlantics C18Chromatographic column (150 mm × 4.6 mm, 5
μm), flowing is acetonitrile-0.5% formic acid solution mutually, uses gradient elution program, and flow velocity is 1 mL/min, and detection wavelength is 276
Nm, under the conditions of being somebody's turn to do, the range of linearity of material is 1 ~ 50 μ g/mL, and recovery of standard addition is more than 95.34%, and relative standard deviation is less than
Between 4.71%.The in a few days RSD of method is less than 4.47%, and RSD is less than 4.79% in the daytime.
This method have easy and simple to handle, accuracy good, highly sensitive, advantages of environment protection, is suitable for spice in rice
Detection.
Claims (5)
1. the method for spice in ionic liquid aqueous two-phase extraction/HPLC detection rice, it is characterised in that include following step
Rapid:
S1. extraction: add [Bmim] Cl/ dipotassium hydrogen phosphate double-aqueous phase system in rice to be measured by the mass ratio of 1:5 ~ 20, mixed
20 ~ 50 DEG C of water-bath 10 ~ 40min after even, phase solution in taking-up；
Wherein, in [Bmim] Cl/ dipotassium hydrogen phosphate double-aqueous phase system, the mass fraction of [Bmim] Cl is 10 ~ 25%, phosphoric acid hydrogen two
The mass fraction of potassium is 30 ~ 50%；
S2.HPLC detects: is diluted by upper phase solution with flowing phase solution, carries out HPLC analysis after filtering with microporous membrane, draws mark
Directrix curve and recovery of standard addition.
Method the most according to claim 1, it is characterised in that in system, the mass fraction of [Bmim] Cl is 15%, phosphoric acid hydrogen
The mass fraction of dipotassium is 35%.
Method the most according to claim 1, it is characterised in that rice to be measured and [Bmim] Cl/ dipotassium hydrogen phosphate aqueous two-phase
The mass ratio of system is 1:10.
Method the most according to claim 1, it is characterised in that HPLC detection uses Atlantis C18Chromatographic column, flow phase
For acetonitrile-0.5% formic acid solution, flow velocity is 1.0 mL/min, and detection wavelength is 276 nm, column temperature 30 DEG C, sample size 10 μ L.
Method the most according to claim 1, it is characterised in that upper phase solution is diluted 2 ~ 5 times with flowing phase solution.
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| CN105445081B (en) * | 2015-11-24 | 2018-06-08 | 长安大学 | The application of vitamin B6 in a kind of double-aqueous phase system and its separation watermelon flesh |
| CN114858939A (en) * | 2022-04-27 | 2022-08-05 | 国家烟草质量监督检验中心 | Method for simultaneously determining eugenol, maltol, ethyl maltol, vanillin and ethyl vanillin in novel atomized product |
Citations (3)
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| CN101164905A (en) * | 2007-10-16 | 2008-04-23 | 中国科学院长春应用化学研究所 | Method for extracting and enriching aromatic compounds in water by double water-phase |
| CN101502722A (en) * | 2008-12-29 | 2009-08-12 | 嘉兴学院 | Ionic liquid double-aqueous phase system for extracting residual antibiotic in foodstuffs and use thereof |
| CN102507833A (en) * | 2011-11-08 | 2012-06-20 | 韩超 | Method for determining vanillin, ethyl vanillin and coumarin in milk by solid phase extraction-liquid chromatogram-electrospray tandem mass spectrometry |
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Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101164905A (en) * | 2007-10-16 | 2008-04-23 | 中国科学院长春应用化学研究所 | Method for extracting and enriching aromatic compounds in water by double water-phase |
| CN101502722A (en) * | 2008-12-29 | 2009-08-12 | 嘉兴学院 | Ionic liquid double-aqueous phase system for extracting residual antibiotic in foodstuffs and use thereof |
| CN102507833A (en) * | 2011-11-08 | 2012-06-20 | 韩超 | Method for determining vanillin, ethyl vanillin and coumarin in milk by solid phase extraction-liquid chromatogram-electrospray tandem mass spectrometry |
Non-Patent Citations (2)
| Title |
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| Extraction of vanillin using ionic-liquid-based aqueous two-phase systems;Ana Filipa M. Cláudio et al;《Separation and Purification Technology》;20100924;第75卷(第1期);第40页"2. 试验"小节和摘要 * |
| HPLC法同时测定烟用添加剂中的香兰素、乙基香兰素、麦芽酚和乙基麦芽酚;任呼博 等;《分析试验室》;20140725;第33卷(第8期);第950-951页"1 实验部分"小节，第952页"2.3 方法的线性范围、相关系数和检出限"和"2.4 样品分析"小节，表4 * |
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