CN115078604A - Pretreatment method for detecting ethanol carbamate in wine - Google Patents
Pretreatment method for detecting ethanol carbamate in wine Download PDFInfo
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- CN115078604A CN115078604A CN202210647894.8A CN202210647894A CN115078604A CN 115078604 A CN115078604 A CN 115078604A CN 202210647894 A CN202210647894 A CN 202210647894A CN 115078604 A CN115078604 A CN 115078604A
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- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
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- G01N30/02—Column chromatography
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- G01N2030/062—Preparation extracting sample from raw material
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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
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- G01N2030/065—Preparation using different phases to separate parts of sample
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Abstract
The invention relates to the technical field of wine detection, and discloses a pretreatment method for detecting ethyl carbamate in wine, which comprises the following steps: (1) adding a certain amount of Fe to the wine sample 3 O 4 Functional magnetic beads, vortex dispersing, standing for adsorption, and separating Fe by magnetic frame 3 O 4 Functional magnetic beads; (2) leaching Fe by using n-hexane 3 O 4 Separating functional magnetic beads by using a magnetic frame, and taking a separation solution; (3) eluting ethyl carbamate with ethyl acetate-diethyl ether solution to obtain eluent; (4) and introducing a proper amount of nitrogen into the eluent, and metering the volume by using methanol to obtain the liquid to be detected. The pretreatment method adopts the MDSPE technology, so that the extraction process is simplified, the treatment cost is low, and secondary pollution is avoided; and the interference of impurities can be avoided, and the ethyl carbamate in the wine can be accurately extracted, so that the detection result is more accurate.
Description
Technical Field
The invention relates to the technical field of liquor detection, in particular to a pretreatment method for detecting ethyl carbamate in liquor.
Background
In recent years, the measurement of the content of urethane in foods has been receiving much attention because excessive presence of urethane in foods adversely affects the quality of foods and threatens human health. In drinks such as wines and the like, the content of the ethyl carbamate is low, so that higher requirements are imposed on detection means and detection technology. At present, the detection and analysis of ethyl carbamate in alcoholic beverages are generally performed by methods such as Gas chromatography-mass spectrometry (GC/MS) detection, two-dimensional or multi-dimensional chromatography-stable isotope dilution mass spectrometry, high performance liquid chromatography combined with fluorescence monitor (HPLC-FLD), Fourier Transform Infrared Spectrometer (FTIR Spectrometer), and the like.
In the method for detecting the content of ethyl carbamate by adopting the instrumental analysis, a wine beverage sample needs to be pretreated, and the pretreatment methods comprise Liquid-Liquid extraction (LLE), Solid Phase Extraction (SPE), Solid Phase Micro Extraction (SPME) and the like. However, the above pretreatment method is complicated in operation process, and the consumption and waste of the organic solvent are large.
In summary, a convenient and efficient sample pretreatment method is urgently needed to determine the content of the ethanol carbamate in the wine.
Disclosure of Invention
The technical problems to be solved by the invention are as follows:
at present, the methods such as LLE, SPE, SPME and the like generally adopted in the pretreatment process for detecting the content of the ethyl carbamate in the wine by adopting methods such as GC-MS, HPLC-FLD, FTIR Spectrometer and the like have the problems of complicated operation steps and large consumption and waste of organic solvents.
The technical scheme adopted by the invention is as follows:
the invention provides a pretreatment method for detecting ethyl carbamate in wine, which comprises the following steps:
(1) taking a proper amount of wine sample, selecting adsorption conditions, and adding a certain amount of Fe 3 O 4 Functional magnetic beads, vortex dispersing, standing for 0.5-2min, and separating Fe with magnetic frame 3 O 4 Functional magnetic beads, taking Fe 3 O 4 Functional magnetic beads;
(2) leaching Fe obtained in (1) with quantitative n-hexane 3 O 4 Separating functional magnetic beads for 10-40s by using a magnetic frame, and taking a separation solution;
(3) eluting the ethyl carbamate with a proper amount of 5% ethyl acetate-diethyl ether solution to obtain an eluent;
(4) and (4) introducing a proper amount of nitrogen into the eluent obtained in the step (3) for concentration, and metering volume by using methanol to obtain a liquid to be detected.
The technical mechanism adopted by the invention is as follows:
magnetic Dispersed Solid Phase Extraction (MDSPE) is a solid phase extraction technique that uses Magnetic or magnetizable materials as an adsorbent matrix. Based on MDSPE technology, the research finds that ethyl carbamate in wine is a magnetic substance, the magnetic effect of the magnetic substance can be utilized, the ethyl carbamate is adsorbed and separated by MDSPE, and the magnetic Fe 3 O 4 Can effectively adsorb the urethane in the wine under the magnetic action, and because the impurity in the wine is mostly diamagnetic material, consequently, can avoid the interference of other impurity substance in the adsorption process.
The beneficial effects of the invention are as follows:
(1) the MDSPE is adopted to simplify the extraction process, expensive equipment is not needed, and trace substances in a large-volume sample can be separated in a short time.
(2) Compared with the existing method, the method has the advantages of obviously reduced consumption of chemical substances, no secondary pollution, and Fe for extraction 3 O 4 The functional magnetic beads are convenient to synthesize.
(3) MDSPE can not only extract target analytes in solution, but also extract target analytes in suspension; because the impurities in the wine sample are generally diamagnetic substances, the interference of the impurities can be effectively avoided.
Detailed Description
In order to make the objects, technical solutions and advantages of the embodiments of the present invention clearer, the technical solutions in the embodiments of the present invention will be clearly and completely described below. The examples, in which specific conditions are not specified, were conducted under conventional conditions or conditions recommended by the manufacturer. The reagents or instruments used are not indicated by the manufacturer, and are all conventional products available commercially.
The invention provides a pretreatment method for detecting ethyl carbamate in wine, which comprises the following steps:
(1) taking a proper amount of wine samples, and selecting adsorption conditions: pH 4-6, temperature 25-35 deg.C, adsorption time 5-15 min; adding a certain amount of Fe 3 O 4 Functional magnetic beads, vortex dispersing, standing for 0.5-2min, and separating Fe with magnetic frame 3 O 4 Functional magnetic beads, taking Fe 3 O 4 Functional magnetic beads;
(2) leaching Fe obtained in (1) with quantitative n-hexane 3 O 4 Separating functional magnetic beads for 10-40s by using a magnetic frame, and taking a separation solution;
(3) eluting the ethyl carbamate with a proper amount of 5% ethyl acetate-diethyl ether solution to obtain an eluent;
(4) and (4) introducing a proper amount of nitrogen into the eluent obtained in the step (3), and metering the volume by using methanol to obtain the liquid to be detected.
Wherein, the wine sample is 1-4g and the magnetic beads are 1-4mg by mass.
In the invention, the liquid to be detected is obtained by adopting Magnetic Dispersed Solid Phase Extraction (MDSPE), so that the extraction process is simplified, the treatment cost is low, and secondary pollution is avoided; and the interference of impurities can be avoided, and the ethanol carbamate in the wine can be accurately extracted, so that the detection result is more accurate.
Secondly, the invention provides Fe adopted by the pretreatment method 3 O 4 The synthesis method of the functional magnetic bead comprises the following steps:
s1 dissolving FeCl in ultrapure water 3 ·6H 2 O and FeCl 2 ·4H 2 Introducing enough ammonia gas to remove oxygen in the solution to obtain reaction liquid;
s2, adding ammonia water into the reaction solution, and reacting for 15-45min at 45-55 ℃;
s3 separating the product obtained after the reaction in S2 with a magnet, washing with ultrapure water, and removing unreacted ammonia water to obtain Fe 3 O 4 Nanoparticles;
s4 for Fe 3 O 4 Surface of nanoparticlesModifying and amination to obtain Fe 3 O 4 Functional magnetic beads;
wherein in S1, the ultrapure water is 120-180mL, and the FeCl 3 ·6H 2 O10-14mmol，FeCl 2 ·4H 2 O5-7 mmol; in S2, the amount of ammonia added was 11-14 mL.
In the invention, the chemical coprecipitation method is adopted to synthesize Fe 3 O 4 And (4) functional magnetic beads. The ammonia gas is introduced into the S1, so that the oxygen can be effectively removed, and the Fe can be avoided 3 O 4 Oxidized in an aerobic environment, affecting the final Fe 3 O 4 And (4) synthesizing functional magnetic beads.
< example 1>
The embodiment provides a pretreatment method for detecting ethyl carbamate in wine, which comprises the following steps:
(1) accurately measuring a 2g wine sample, and selecting adsorption conditions: pH 5, temperature 30 deg.C, adsorption time 10 min; 2mg of Fe was added 3 O 4 Functional magnetic beads, vortex dispersing, standing for 1min, and separating Fe with magnetic frame 3 O 4 Functional magnetic beads, taking Fe 3 O 4 Functional magnetic beads;
(2) leaching Fe obtained in (1) with 2mL of n-hexane 3 O 4 Separating functional magnetic beads for 30s by using a magnetic frame, and taking a separation solution;
(3) eluting the ethyl carbamate with 2mL of 5% ethyl acetate-diethyl ether solution to obtain an eluent;
(4) and (4) blowing nitrogen into the eluent obtained in the step (3) to about 0.5mL, and metering the volume to 1mL by using methanol to obtain a solution to be detected.
This example provides a Fe used in the pretreatment method 3 O 4 The method for synthesizing the functional magnetic beads comprises the following steps:
s1 in 150mL of ultrapure water, 11.2mmol of FeCl was dissolved 3 ·6H 2 O and 5.6mmol FeCl 2 ·4H 2 Introducing sufficient ammonia gas to obtain reaction liquid;
s2 adding 12.5mL ammonia water into the reaction solution, reacting for 30min at 50 ℃;
s3 magnetic treatment of the product obtained after the reaction in S2Separating iron, washing with ultrapure water, removing unreacted ammonia water to obtain Fe 3 O 4 Nanoparticles;
s4 for Fe 3 O 4 The surface modification of the nano particles is carried out for amination to obtain Fe 3 O 4 And (4) functional magnetic beads.
Wherein, ammonia gas is introduced into S1 to remove oxygen and avoid Fe 3 O 4 Is oxidized.
< example 2>
This example differs from example 1 in that in step (1) the amount of wine sample taken was 4g, Fe 3 O 4 The amount of the functional magnetic beads added was 1 mg.
< example 3>
The difference between this example and example 1 is that in step (1), the adsorption conditions are selected as follows: pH 6, temperature 25 ℃, adsorption time 5 min.
< example 4>
This example differs from example 1 in that in step S1, 14mmolFeCl is dissolved 3 ·6H 2 O and 5mmolFeCl 2 ·4H 2 O。
< example 5>
This example differs from example 4 in that 10mmol of FeCl was dissolved in step S1 3 ·6H 2 O and 5mmolFeCl 2 ·4H 2 O。
< comparative example 1>
In this comparative example, the Liquid to be detected was prepared by conventional Liquid-Liquid extraction (LLE).
< comparative example 2>
In this comparative example, the liquid to be detected was prepared by conventional Solid Phase Extraction (SPE).
< comparative example 3>
In this comparative example, the liquid to be detected was prepared by conventional Solid Phase Micro Extraction (SPME).
< test example >
The samples in the examples 1 to 5 and the comparative examples 1 to 3 are subjected to GC/MS analysis, each group of samples is subjected to component analysis by a plurality of groups of parallel experiments, in the analysis pretreatment stage, the time spent in the examples 1 to 5 is shorter, the steps are simpler and more convenient, and the analysis results of the examples 1 to 5 and the comparative examples 1 to 3 are very little different, so that the pretreatment operation can be obviously simplified and the pretreatment efficiency can be effectively improved by adopting the pretreatment method of the examples 1 to 5 on the basis of ensuring the accuracy of the results.
The above description is only a preferred embodiment of the present invention and is not intended to limit the present invention, and various modifications and changes may be made by those skilled in the art. Any modification, equivalent replacement, or improvement made within the spirit and principle of the present invention should be included in the protection scope of the present invention.
Claims (7)
1. A pretreatment method for detecting ethanol carbamate in wine is characterized by comprising the following steps:
(1) taking wine sample, selecting adsorption condition, adding Fe 3 O 4 Functional magnetic beads, vortex dispersing, standing for adsorption, and separating Fe by magnetic frame 3 O 4 Functional magnetic beads, taking Fe 3 O 4 Functional magnetic beads;
(2) leaching Fe obtained in step (1) with n-hexane 3 O 4 Separating functional magnetic beads by using a magnetic frame, and taking a separation solution;
(3) eluting the ethyl carbamate with ethyl acetate-diethyl ether solution to obtain an eluent;
(4) and (4) introducing a proper amount of nitrogen into the eluent obtained in the step (3), and metering the volume by using methanol to obtain the liquid to be detected.
2. The pretreatment method for detecting ethanol carbamate in wine as claimed in claim 1, wherein in the step (1), the wine sample is 500-2000 parts by weight of Fe 3 O 4 0.5-2 parts of functional magnetic beads.
3. The pretreatment method for detecting ethanol carbamate in wine according to claim 1, wherein in the step (1), the adsorption conditions are selected as follows: pH 4-6, temperature 25-35 deg.C, and adsorption time 5-15 min.
4. The pretreatment method for detecting ethanol carbamate in wine according to claim 1, comprising the steps of:
(1) accurately weighing 1-4g wine sample, adding 1-4mg Fe 3 O 4 Functional magnetic beads, vortex dispersing, standing for 0.5-2min, and separating Fe with magnetic frame 3 O 4 Functional magnetic beads, taking Fe 3 O 4 Functional magnetic beads;
(2) leaching Fe obtained in step (1) with quantitative n-hexane 3 O 4 Separating functional magnetic beads for 10-40s by using a magnetic frame, and taking a separation solution;
(3) eluting the ethyl carbamate with a proper amount of 5% ethyl acetate-diethyl ether solution to obtain an eluent;
(4) and (4) introducing about 0.5mL of eluent obtained in the step (3), and metering the volume to 1mL by using methanol to obtain a liquid to be detected.
5. Fe as claimed in any one of claims 1 to 4 3 O 4 The method for synthesizing the functional magnetic beads is characterized by comprising the following steps of:
s1 dissolving FeCl in ultrapure water 3 ·6H 2 O and FeCl 2 ·4H 2 Introducing ammonia gas to obtain a reaction solution;
s2, adding ammonia water into the reaction solution, and reacting for 15-45min at 45-55 ℃;
s3 separating the product obtained after the reaction in S2 with a magnet, washing with ultrapure water, and removing unreacted ammonia water to obtain Fe 3 O 4 Nanoparticles;
s4 for Fe 3 O 4 The surface modification of the nano particles is carried out for amination to obtain Fe 3 O 4 And (4) functional magnetic beads.
6. The pretreatment method for detecting ethanol carbamate in wine according to claim 5, wherein the pretreatment method comprises the step of adding FeCl into the wine according to the molar mass 3 ·6H 2 O is 2 parts, FeCl 2 ·4H 2 0.8-1.2 parts of O.
7. The pretreatment method for detecting ethanol carbamate in wine according to claim 5, comprising the steps of:
s1 dissolving FeCl in ultrapure water 3 ·6H 2 O and FeCl 2 ·4H 2 Introducing ammonia gas to obtain a reaction solution;
s2, adding a certain amount of ammonia water into the reaction solution, and reacting for 30min at 50 ℃;
s3 separating the product obtained after the reaction in S2 by using a magnet, washing the product with ultrapure water, and removing unreacted ammonia water to obtain Fe 3 O 4 Nanoparticles;
s4 for Fe 3 O 4 The surface modification of the nano particles is carried out for amination to obtain Fe 3 O 4 And (4) functional magnetic beads.
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