CN111257443B - Method for detecting sudan red dye in fruit and vegetable juice - Google Patents
Method for detecting sudan red dye in fruit and vegetable juice Download PDFInfo
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- CN111257443B CN111257443B CN202010058628.2A CN202010058628A CN111257443B CN 111257443 B CN111257443 B CN 111257443B CN 202010058628 A CN202010058628 A CN 202010058628A CN 111257443 B CN111257443 B CN 111257443B
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- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
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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
- G01N30/08—Preparation using an enricher
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Abstract
The invention relates to the field of food safety, in particular to a method for detecting sudan red dye in fruit and vegetable juice, which is used for preparing a magnetic porous carbon nanofiber material with large specific surface area and porous structure; the invention uses the magnetic porous carbon nanofiber material for magnetic solid-phase adsorption extraction of Sudan red dye in fruit and vegetable juice, and finally uses a High Performance Liquid Chromatography (HPLC) serial PDA detector to analyze and detect the Sudan dye. The method has the advantages of simple operation, high extraction efficiency, small using amount of the organic solvent, high sensitivity and the like.
Description
Technical Field
The invention relates to the field of food safety, in particular to a detection method of a sudan red dye in fruit and vegetable juice.
Background
In recent years, the economic level of China is remarkably improved, the life quality of people is also greatly improved, and the importance of food safety is also increased year by year.
Sudan red dye is an artificially synthesized azo dye, and because of the special chemical structure, the metabolic products of the compound have obvious toxicity to organs such as skin, liver, kidney and the like of a human body, and are classified as tertiary carcinogens. Sudan red dyes are commonly used in industrial printing and dyeing, such as shoe polish, floor color enhancement, and the like.
Because of the complex food matrix and low analyte levels, sample pretreatment of the analyte is often required. The most commonly used sample pretreatment method for detecting sudan red at present is (1) extracting sudan red dye in food by using normal hexane, and (2) enriching and purifying by using a solid phase extraction column, and detecting after concentrating the obtained eluent. Because the extraction efficiency of n-hexane is lower in the treatment process, a large amount of organic solvent is used, and the solid phase extraction of the small column takes a long time, the method is complex in operation and the recovery rate is usually low.
Disclosure of Invention
The invention aims to provide a method for detecting sudan red dye in fruit and vegetable juice, which is simple in preparation method, simple and convenient in operation in the sample pretreatment process, and capable of effectively avoiding the interference of complex matrixes in the detection process, improving the enrichment factor and improving the detection sensitivity.
A detection method of a sudan red dye in fruit and vegetable juice comprises the following steps: (1) Dissolving 1.0-3.0 g PAN and 0.1-0.5 g PMMA in DMF, heating the solution to 50-70 ℃, stirring and reacting for 12 hours, and passing through an electrostatic spinning methodSpinning the solution obtained by the reaction and obtaining a nanofiber material, placing the nanofiber obtained by the spinning in a vacuum drying oven at 50-70 ℃ for drying for 24 hours, placing the dried nanofiber material in a tubular furnace, setting the temperature of the tubular furnace to 280 ℃ and keeping for 4 hours, introducing argon, setting a temperature program to 1000 ℃, obtaining a porous carbon nanofiber material, and grinding for later use; (2) Taking the porous carbon nanofiber material prepared in the step (1), dispersing the porous carbon nanofiber material in an aqueous solution by ultrasonic, maintaining a nitrogen environment, and adding FeCl 3 ·6H 2 O and FeCl 2 ·4H 2 O, heating to 70 ℃, adding ammonia water solution dropwise to adjust the pH value to 10, keeping the temperature at 70 ℃, stirring and reacting for 1 hour, collecting the magnetic porous carbon nanofiber by a magnet, alternately washing the magnetic porous carbon nanofiber with ethanol and water for multiple times, and drying in a vacuum drying oven for later use.
In one example, in step (1) 2.0g and 0.4g of PAN and PMMA are dissolved in DMF, respectively, the solution is heated to 60℃and the nanofibers are dried in a vacuum oven at 60℃for 24 hours.
The application of the magnetic porous carbon nanofiber prepared by the preparation method in detecting the sudan red dye in fruit and vegetable juice.
In one embodiment, the method comprises the following steps: (1) Adding 10mL of commercial fruit and vegetable juice into a centrifuge tube, adding 1-6 mg of the magnetic porous carbon nanofiber, adding 0.1-1.0 g of NaCl, shaking and uniformly mixing for 5-30 min, adsorbing a solid-phase adsorbent by using a magnet, pouring the extracted liquid, and eluting the adsorbent by using one of methanol, ethanol or acetonitrile; (2) evaporating the eluent under reduced pressure to obtain residue; (3) The residue was redissolved in 200. Mu.L of acetonitrile and filtered through a 0.22 μm organic filter membrane before being injected into HPLC for determination.
In one embodiment, the magnetic porous carbon nanofiber added in the step (1) is 3mg, the added NaCl is 0.8g, the shaking and mixing time is 15min, and the used eluting solvent is 4mL of ethanol. The beneficial effects of the invention are as follows:
the magnetic porous carbon nanofiber prepared by the invention has the characteristics of porous structure, large specific surface area and high adsorption capacity, can be reused, has the advantage of enriching trace compounds, is combined with magnetic solid phase extraction, and has the advantages of simple operation and short analysis time; the pretreatment of the sample related by the invention does not need centrifugal operation, and the equipment is simple; the detection limit of Sudan I, sudan II, sudan III, sudan IV and Sudan red 7B in the invention is low, the repeatability is good and the sensitivity is high.
Drawings
FIG. 1 is an SEM image and a TEM image of a magnetic porous carbon nanofiber;
FIG. 2 is a flow chart of a solid phase adsorbent preparation process and a magnetic solid phase extraction process;
FIG. 3 is a chromatogram of an untreated fruit and vegetable juice sample detected at wavelengths 478nm, 520nm and 538nm and a chromatogram after magnetic solid phase extraction.
Detailed Description
The present invention will be further described in detail with reference to the drawings and the detailed description, in order to make the objects, technical solutions and advantages of the present invention more apparent. It should be understood that the detailed description and specific examples are intended for purposes of illustration only and are not intended to limit the scope of the invention.
In the present invention, unless otherwise specified, all equipment and materials are commercially available or are commonly used in the industry, and the methods in the examples are conventional in the art unless otherwise specified.
Example 1
Preparation of magnetic porous carbon nanofiber
(1) 2.0g of PAN and 0.4g of PMMA are taken and dissolved in DMF, the solution is heated to 60 ℃, stirred and reacted for 12 hours, the solution obtained by the reaction is spun through an electrostatic spinning method and a nanofiber material is obtained, the nanofiber obtained by spinning is placed in a vacuum drying oven at 60 ℃ and dried for 24 hours, the dried nanofiber material is placed in a tube furnace, the temperature of the tube furnace is set to 280 ℃ and kept for 4 hours, argon is introduced, the temperature programming is set to 1000 ℃, and the porous carbon nanofiber material is obtained, and is ground for standby;
(2) Taking the porous carbon nano prepared in the step (1)Dispersing fiber material in water solution by ultrasonic wave, maintaining nitrogen environment, adding FeCl 3 ·6H 2 O and FeCl 2 ·4H 2 O, heating to 70 ℃, adding ammonia water solution dropwise to adjust the pH value to 10, keeping the temperature at 70 ℃, stirring and reacting for 1 hour, collecting the magnetic porous carbon nanofiber by a magnet, alternately washing the magnetic porous carbon nanofiber with ethanol and water for multiple times, and drying in a vacuum drying oven for later use.
The structure of the magnetic porous nanofiber material was examined by scanning electron microscopy and transmission electron microscopy, and the results of the examination are shown in fig. 1.
Example 2
Application of magnetic porous carbon nanofiber in detecting Sudan red dye in fruit and vegetable juice is shown in fig. 2-3.
(1) Taking 10mL of commercial fruit and vegetable juice in a centrifuge tube, adding 3mg of the magnetic porous carbon nanofiber, adding 0.8g of NaCl, shaking and uniformly mixing for 15min, adsorbing a solid-phase adsorbent by using a magnet, pouring the extracted liquid, and eluting the adsorbent by using 4mL of ethanol;
(2) Evaporating the eluent under reduced pressure to dryness to obtain residues;
(3) The residue was redissolved in 200. Mu.L of acetonitrile and filtered through a 0.22 μm organic filter membrane before being injected into HPLC for determination.
The detection results of the untreated fruit and vegetable juice samples and the fruit and vegetable juice samples after the magnetic solid phase extraction are shown in the specification, wherein 1 to 5 in the figure 3 represent Sudan I, sudan II, sudan III, sudan red 7B and Sudan IV respectively.
Sudan I, sudan II, sudan III, sudan IV and Sudan red 7B have detection limits of 0.90 mug/L, 1.39 mug/L, 0.92 mug/L, 1.28 mug/L and 1.46 mug/L respectively, daily precision RSD values of 2.4%, 3.2%, 1.8%, 2.5% and 2.7% respectively, daily precision RSD values of 3.8%, 5.3%, 2.2%, 2.8% and 4.2% respectively, and sample recovery rates of 97.7%, 95.4%, 94.9%, 86.3% and 83.4% respectively.
Claims (3)
1. The method for detecting the sudan red dye in the fruit and vegetable juice is characterized by comprising the following steps of: (1) Adding 10mL commercial fruit and vegetable juice into a centrifuge tube, adding 1-6 mg magnetic porous carbon nanofibers, adding 0.1-1.0 g NaCl, shaking and uniformly mixing for 5-30 min, adsorbing a solid-phase adsorbent by using a magnet, pouring the extracted liquid, and eluting the adsorbent by using one of methanol, ethanol or acetonitrile; (2) evaporating the eluent under reduced pressure to dryness to obtain residues; (3) The residue was redissolved in 200 μl acetonitrile and filtered through a 0.22 μm organic filter membrane, and then injected into HPLC for determination; the preparation method of the magnetic porous carbon nanofiber comprises the following steps: (A) Dissolving 1.0-3.0 g of PAN and 0.1-0.5 g of PMMA in DMF, heating the solution to 50-70 ℃, stirring and reacting for 12 hours, spinning the solution obtained by the reaction by an electrostatic spinning method to obtain a nanofiber material, drying the nanofiber material obtained by spinning in a vacuum drying box at 50-70 ℃ for 24 hours, placing the dried nanofiber material in a tubular furnace, setting the temperature of the tubular furnace to 280 ℃ and keeping for 4 hours, introducing argon, setting a program to rise to 1000 ℃, finally obtaining a porous carbon nanofiber material, and grinding for later use; (B) And (3) taking the porous carbon nanofiber material prepared in the step (A), dispersing the porous carbon nanofiber material in an aqueous solution in an ultrasonic manner, maintaining a nitrogen environment, adding FeCl3.6H2O and FeCl2.4H2O, heating to 70 ℃, adding an ammonia water solution dropwise to adjust the pH value to 10, maintaining the temperature at 70 ℃, stirring and reacting for 1 hour, collecting the obtained magnetic porous carbon nanofiber material through a magnet, alternately washing the obtained magnetic porous carbon nanofiber material with ethanol and water for multiple times, and drying the obtained magnetic porous carbon nanofiber material in a vacuum drying box for later use.
2. The method of claim 1, wherein PAN and PMMA are dissolved in DMF at 2.0. 2.0g and 0.4. 0.4g, respectively, the solution is heated to 60 ℃, and the nanofiber material is dried in a vacuum oven at 60 ℃ for 24 hours.
3. The method for detecting sudan red dye in fruit and vegetable juice according to claim 1, wherein the magnetic porous carbon nanofiber added in the step (1) is 3mg, the NaCl added is 0.8g, the shaking and mixing time is 15min, and the used eluting solvent is 4mL ethanol.
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102253139A (en) * | 2011-06-14 | 2011-11-23 | 吉林大学 | Method for detecting tonyred concentration in environment water sample |
| CN103645177A (en) * | 2013-12-23 | 2014-03-19 | 武汉大学 | Method for improving Sudan red I detection kit |
| CN110158237A (en) * | 2019-04-30 | 2019-08-23 | 苏州大学 | A kind of preparation method and application of the porous carbon nanofiber film of rapid heavy metal ion adsorption |
Family Cites Families (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US9353137B2 (en) * | 2014-02-07 | 2016-05-31 | Ghassem Amoabediny | Method for separation and purification of phosphatidylcholine employing magnetic nanoparticles and compositions so produced |
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- 2020-01-19 CN CN202010058628.2A patent/CN111257443B/en active Active
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102253139A (en) * | 2011-06-14 | 2011-11-23 | 吉林大学 | Method for detecting tonyred concentration in environment water sample |
| CN103645177A (en) * | 2013-12-23 | 2014-03-19 | 武汉大学 | Method for improving Sudan red I detection kit |
| CN110158237A (en) * | 2019-04-30 | 2019-08-23 | 苏州大学 | A kind of preparation method and application of the porous carbon nanofiber film of rapid heavy metal ion adsorption |
Non-Patent Citations (7)
| Title |
|---|
| Carbon nanofibers decorated with magnetic nanoparticles as a new sorbent for the magnetic solid phase extraction of selected polycyclic aromatic hydrocarbons from water samples;Ali Sarafraz-Yazdi 等;New J. Chem;第39卷;第3.1-3.2节 * |
| Fe_3O_4-β-环糊精聚合物固相萃取紫外可见光谱法分离分析孔雀石绿;冯刚;平文卉;朱霞石;;光谱学与光谱分析(02);436-441 * |
| Synthesis of mesoporous magnetic Fe3O4@carbon nanofibers utilizing in situ polymerized polybenzoxazine for water purification;Yang Si 等;Journal of Materials Chemistry;第22卷;4619-4622 * |
| β-环糊精功能化聚丙烯腈纳米纤维的制备及对亚甲基蓝的吸附性能;张旺;陈铭;刁国旺;;高等学校化学学报(09);2227-2230 * |
| 聚合物共混制备纳米和多孔碳纤维及性能研究;谢天时;端小平;李光;;材料导报(12);97-100 * |
| 苏丹红Ⅰ磁性分子印迹聚合物的制备及其分离分析应用;马洁;黄静;曾延波;张祖磊;张剑;陈智栋;李蕾;;分析测试学报(06);726-731 * |
| 静电纺丝法制备的多孔碳纳米纤维;李静 等;电池;第41卷(第3期);第1.1-1.2节 * |
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