CN107192772B - Method for detecting 3-acetyl-2,5-dimethylthiophene - Google Patents
Method for detecting 3-acetyl-2,5-dimethylthiophene Download PDFInfo
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Abstract
The invention discloses a method for detecting 3-acetyl-2,5-dimethylthiophene by combining acid-base induction liquid-liquid microextraction with magnetic solid-phase purification high performance liquid chromatography. The method comprises the steps of adding a mixture of fatty acid and nonionic surfactant into a detected liquid containing 3-acetyl-2,5-dimethylthiophene, adding a mixture of alkali, fatty acid and nonionic surfactant to form a homogeneous micelle, extracting 3-acetyl-2,5-dimethylthiophene, adding acid to induce phase separation, wherein the mixture of 3-acetyl-2,5-dimethylthiophene, fatty acid and nonionic surfactant has good affinity, and the extraction rate exceeds 98%; reuse of magnetic Fe3O4The nano particles purify the sample, and the content of the nano particles is determined by combining high performance liquid chromatography. Magnetic Fe3O4The nano particles can well adsorb fat coexisting with the 3-acetyl-2,5-dimethylthiophene in a sample, and the interference of the nano particles on detection is eliminated. The extraction technology is carried out at room temperature, extraction is completed within 20min, and the method has the characteristics of simple and convenient operation, rapidness, high sensitivity and the like, and the detection sensitivity of the method reaches 0.5 mu g/kg.
Description
Technical Field
The invention belongs to the field of analytical chemistry, and particularly relates to a method for detecting 3-acetyl-2,5-dimethylthiophene by combining acid-base induction liquid-liquid microextraction and magnetic solid-phase purification with high performance liquid chromatography.
Background
3-acetyl-2,5-dimethylthiophene is used as a food essence additive, the aroma of the food essence additive has the smell of mildew and rot like vegetable roots, the aroma of nuts, a slightly baked aroma and the aroma of poultry meat. The product can be widely used in sesame, potato, walnut, grape, mushroom, vegetable, ginseng, tropical fruit and meat essence. On the 15 th 6 th month in 2013, committee regulation No. 545/2013 issued by the european union, regulation No. 1334/2008 on flavor and fragrance, and 3-acetyl-2,5-dimethylthiophene (3-acetyl-2, 5-dimethylthiophane, FEMA 3527) as a flavor for food are prohibited. In 14/8/2014, the association of the flavor and fragrance cosmetics industry in China issued a flavor and fragrance industry discipline document-a restriction requirement on 3-acetyl-2,5-dimethylthiophene (xianghua xie [2013] No. 62), and the discipline document regulation, according to the existing safety assessment conclusion and the investigation result of the association on the production and use conditions of 3-acetyl-2,5-dimethylthiophene in some flavor and fragrance major production enterprises in China: since the date of the release of this autonomous document, 3-acetyl-2,5-dimethylthiophene used as a flavor for food cannot be produced by flavor manufacturing enterprises; the food essence production enterprise adjusts the formula and can not use the substance.
At present, no detection method for 3-acetyl-2,5-dimethylthiophene in food additives exists in China, and related researches are lacked. The invention discloses a method for determining 3-acetyl-2,5-dimethylthiophene in a food additive (CN 104655753A), which discloses a method for determining 3-acetyl-2,5-dimethylthiophene in the food additive by using an internal standard gas chromatography-mass spectrometry.
According to the invention, the mixture of fatty acid and nonionic surfactant has better affinity with 3-acetyl-2,5-dimethylthiophene, a homogeneous micelle system is formed by the mixture of alkali, fatty acid and nonionic surfactant and water for the first time, and the 3-acetyl-2,5-dimethylthiophene is extracted efficiently, quickly and simply and conveniently by adding acid to induce phase separation; while utilizing magnetic Fe3O4The nano particles purify the sample, and the content of the nano particles is determined by combining high performance liquid chromatography. Magnetic Fe3O4The nano particles can well adsorb fat coexisting with the 3-acetyl-2,5-dimethylthiophene in a sample, and the interference of the nano particles on detection is eliminated. The extraction technology is carried out at room temperature, extraction is completed within 20min, and the method has the characteristics of simple and convenient operation, rapidness, high sensitivity and the like, the detection sensitivity of the method reaches 0.5 mu g/kg, and the extraction recovery rate reaches 98%.
Disclosure of Invention
The invention aims to provide a method for detecting 3-acetyl-2,5-dimethylthiophene by combining acid-base induction liquid-liquid microextraction and magnetic solid-phase purification with high performance liquid chromatography.
A method for detecting 3-acetyl-2,5-dimethylthiophene by combining acid-base induction liquid-liquid microextraction and magnetic solid-phase purification with high performance liquid chromatography. The method is realized by the following scheme:
adding deionized water 5 times the volume ratio of 3-acetyl-2,5-dimethylthiophene into the extractive solution, and adding magnetic Fe3O4Mixing the nano particles by vortex, carrying out solid-liquid separation by using an external magnetic field, and taking out supernatant; adding a mixture of fatty acid and nonionic surfactant, mixing by vortex to form turbid solution, adding ammonia water, mixing by vortex to form uniform micelle, adding hydrochloric acid, mixing by vortex, centrifuging for phase separation, taking out the mixture of upper fatty acid and nonionic surfactant, and performing content determination by high performance liquid chromatography.
The extracting solution containing 3-acetyl-2,5-dimethylthiophene is obtained by the following method: for solid essence, weighing a certain amount of essence sample, and adding the essence sample in a weight ratio of 1: performing ultrasonic extraction on 10-15 parts of acetone for 30-45min, blowing nitrogen to 1-3 mL, and performing constant volume treatment on the nitrogen to 10mL by using deionized water for later use; and for the liquid essence, 1-3 mL of the liquid essence is taken, and deionized water is added to the liquid essence until the volume is 10mL for later use.
The fatty acid is any one of nonanoic acid, heptanoic acid and octanoic acid, the nonionic surfactant is TMN-6, and the ratio of the fatty acid to the nonionic surfactant is 5: 1, the dosage is 0.2-0.5 mL of the sample solution per 10 mL.
The dosage of the ammonia water is 0.3-0.6 mL added in each 10mL of sample liquid.
The dosage of the hydrochloric acid is 1-2 mL added in each 10mL of sample liquid.
The magnetic Fe3O4The dosage of the nano particles is 5-10 mg added in each 10mL of sample liquid.
The vortex time is 1-3 min.
The centrifugal rotating speed is 3000-5000 r/min, and the time is 5-10 min.
The high performance liquid chromatography conditions are as follows: mobile phase: isocratic elution of methanol-water solution, methanol-water ratio of 65:35, detection wavelength: 296nm, column temperature: 25 ℃, flow rate: 1 mL/min.
Compared with the prior art, the invention has the following remarkable advantages:
1. the mixture of fatty acid and nonionic surfactant has better affinity with 3-acetyl-2,5-dimethylthiophene, a homogeneous micelle system is formed by the mixture of alkali, fatty acid and nonionic surfactant and water for the first time, and then the 3-acetyl-2,5-dimethylthiophene is extracted efficiently, quickly and simply and conveniently by adding acid to induce phase separation.
2. Using magnetic Fe3O4The nano particles purify the sample, and the content of the nano particles is determined by combining high performance liquid chromatography. Magnetic Fe3O4The nano particles can well adsorb fat coexisting with the 3-acetyl-2,5-dimethylthiophene in a sample, and the interference of the nano particles on detection is eliminated.
3. The extraction technology is carried out at room temperature, extraction is completed within 20min, and the method has the characteristics of simple and convenient operation, rapidness, high sensitivity and the like, the detection sensitivity of the method reaches 0.5 mu g/kg, and the extraction recovery rate reaches 98%.
Description of the drawings:
FIG. 1 is a schematic diagram of the acid-base induction liquid-liquid microextraction mechanism involved in the present invention.
Detailed Description
The invention is further illustrated with reference to the following examples, without limiting the scope of the invention thereto.
Example 1: determination of 3-acetyl-2,5-dimethylthiophene in potato essence
(1) Sample preparation: adding deionized water into 1mL of potato essence to a constant volume of 10mL to obtain a sample solution;
(2) and (3) sample determination: adding 5mg of magnetic Fe into the sample solution obtained in the step (1)3O4Mixing nanoparticles for 1min by vortex, performing solid-liquid separation by using an external magnetic field, and taking out supernatant; adding a mixed solution consisting of 500 mu L of caprylic acid and 100 mu L of TMN-6, carrying out vortex mixing for 1min to form a turbid solution, adding 300 mu L of ammonia water, carrying out vortex mixing for 1min to form uniform micelles, adding 1.5mL of hydrochloric acid, carrying out vortex mixing for 2min, centrifuging for 8min at 4000r/min, taking out a mixture of upper layer caprylic acid and nonionic surfactant TMN-6, filtering by a 0.45 mu m organic phase filter membrane, and analyzing by HPLC, wherein the HPLC chromatographic conditions are as follows: mobile phase: isocratic elution of methanol-water solution, methanol-water ratio of 65:35, detection wavelength: 296nm, column temperature: 25 ℃, flow rate: 1 mL/min. The content of 3-acetyl-2,5-dimethylthiophene was measured to be 12.5. mu.g/g.
Example 2: determination of 3-acetyl-2,5-dimethylthiophene in grape essence
(1) Sample preparation: taking 2mL of grape essence, adding deionized water to a constant volume of 10mL to obtain a sample solution;
(2) and (3) sample determination: adding 6mg of magnetic Fe into the sample solution obtained in the step (1)3O4Mixing nanoparticles for 2min by vortex, performing solid-liquid separation by using an external magnetic field, and taking out supernatant; adding 500 μ L of mixed solution of pelargonic acid and 100 μ L of TMN-6, vortex mixing for 2min to form turbid solution, adding 400 μ L of ammonia water, vortex mixing for 1min to form uniform micelle, adding 1mL of hydrochloric acid, vortex mixing for 1min, centrifuging at 3000r/min for 10min, and taking out the mixture of pelargonic acid on the upper layer and non-ionic surfactant TMN-6The resulting product was filtered through a 0.45-. mu.m organic phase filter and analyzed by HPLC under the same conditions as in example 1, whereby the content of 3-acetyl-2,5-dimethylthiophene was 24.6. mu.g/g.
Example 3: determination of 3-acetyl-2,5-dimethylthiophene in beef flavor
(1) Sample preparation: weighing 2g of beef essence, adding 20g of acetone, carrying out ultrasonic extraction for 30min, blowing nitrogen to 1mL, and carrying out constant volume treatment to 10mL with deionized water for later use;
(2) and (3) sample determination: and (3) sample determination: adding 8mg of magnetic Fe into the sample solution obtained in the step (1)3O4Mixing nanoparticles for 3min by vortex, performing solid-liquid separation by using an external magnetic field, and taking out supernatant; adding 500 mu L of mixed solution of heptanoic acid and 100 mu L of TMN-6, carrying out vortex mixing for 2min to form turbid solution, adding 500 mu L of ammonia water, carrying out vortex mixing for 2min to form uniform micelle, adding 2mL of hydrochloric acid, carrying out vortex mixing for 3min, centrifuging for 5min at 5000r/min, taking out the mixture of the upper layer heptanoic acid and the nonionic surfactant TMN-6, filtering by a 0.45 mu m organic phase filter membrane, analyzing by HPLC, and measuring the content of 3-acetyl-2,5-dimethylthiophene by 39.0 mu g/g under the same chromatographic conditions as example 1.
Example 4: determination of 3-acetyl-2,5-dimethylthiophene in pork essence
(1) Sample preparation: weighing 2g of chicken essence, adding 30g of acetone, carrying out ultrasonic extraction for 45min, blowing nitrogen to 3mL, and carrying out constant volume treatment to 10mL with deionized water for later use;
(2) and (3) sample determination: and (3) sample determination: adding 10mg of magnetic Fe into the sample solution obtained in the step (1)3O4Mixing nanoparticles for 3min by vortex, performing solid-liquid separation by using an external magnetic field, and taking out supernatant; adding 500 mu L of mixed solution of octanoic acid and 100 mu L of TMN-6, carrying out vortex mixing for 2min to form turbid solution, adding 600 mu L of ammonia water, carrying out vortex mixing for 2min to form uniform micelle, adding 2mL of hydrochloric acid, carrying out vortex mixing for 3min, centrifuging for 6min at 4500r/min, taking out the mixture of upper octanoic acid and nonionic surfactant TMN-6, filtering by a 0.45 mu m organic phase filter membrane, analyzing by HPLC, and measuring the content of 3-acetyl-2,5-dimethylthiophene by 99.3 mu g/g under the chromatographic conditions same as example 1.
The acid-base induction liquid-liquid micro-extraction mechanism related to the invention is shown in figure 1. The extraction technology is carried out at room temperature, extraction is completed within 20min, and the method has the characteristics of simple and convenient operation, rapidness, high sensitivity and the like, the detection sensitivity of the method reaches 0.5 mu g/kg, and the extraction recovery rate reaches 98%.
Claims (10)
1. A method for detecting 3-acetyl-2,5-dimethylthiophene is characterized by comprising the following steps: adding deionized water 5 times the volume ratio of 3-acetyl-2,5-dimethylthiophene into the extractive solution, and adding magnetic Fe3O4Mixing the nano particles by vortex, carrying out solid-liquid separation by using an external magnetic field, and taking out supernatant; adding a mixture of fatty acid and a nonionic surfactant, carrying out vortex mixing to form a turbid solution, adding ammonia water, carrying out vortex mixing to form a uniform micelle, adding hydrochloric acid, carrying out vortex mixing, carrying out centrifugal phase separation, taking out the mixture of the upper layer of fatty acid and the nonionic surfactant, and carrying out content determination by adopting high performance liquid chromatography; the fatty acid is any one of pelargonic acid, heptanoic acid and caprylic acid; the non-ionic surfactant is TMN-6.
2. The method for detecting 3-acetyl-2,5-dimethylthiophene according to claim 1, wherein: the extracting solution containing 3-acetyl-2,5-dimethylthiophene is obtained by the following method: for solid essence, weighing a certain amount of essence sample, and adding the essence sample in a weight ratio of 1: performing ultrasonic extraction on 10-15 parts of acetone for 30-45min, blowing nitrogen to 1-3 mL, and performing constant volume treatment on the nitrogen to 10mL by using deionized water for later use; and for the liquid essence, 1-3 mL of the liquid essence is taken, and deionized water is added to the liquid essence until the volume is 10mL for later use.
3. The method for detecting 3-acetyl-2,5-dimethylthiophene according to claim 1, wherein: the ratio of fatty acid to nonionic surfactant is 5: 1.
4. the method for detecting 3-acetyl-2,5-dimethylthiophene according to claim 1, wherein: the dosage of the ammonia water is 0.3-0.6 mL added in each 10mL of sample liquid.
5. The method for detecting 3-acetyl-2,5-dimethylthiophene according to claim 1, wherein: the dosage of the hydrochloric acid is 1-2 mL added in each 10mL of sample liquid.
6. The method for detecting 3-acetyl-2,5-dimethylthiophene according to claim 1, wherein: the magnetic Fe3O4The amount of nanoparticles was 5 ~ 10mg per 10mL of sample.
7. The method for detecting 3-acetyl-2,5-dimethylthiophene according to claim 1, wherein said vortex time is 1 ~ 3 min.
8. The method for detecting 3-acetyl-2,5-dimethylthiophene according to claim 1, wherein said centrifugation is performed at 3000 ~ 5000r/min for 5 ~ 10 min.
9. The method for detecting 3-acetyl-2,5-dimethylthiophene according to claim 1, wherein: the high performance liquid chromatography conditions are as follows: mobile phase: isocratic elution of methanol-water solution, methanol-water ratio of 65:35, detection wavelength: 296nm, column temperature: 25 ℃, flow rate: 1 mL/min.
10. The method for detecting 3-acetyl-2,5-dimethylthiophene according to claim 1, wherein: the extracting solution containing 3-acetyl-2,5-dimethylthiophene is obtained by the following method: for solid essence, weighing a certain amount of essence sample, and adding the essence sample in a weight ratio of 1: performing ultrasonic extraction on 10-15 parts of acetone for 30-45min, blowing nitrogen to 1-3 mL, and performing constant volume treatment on the nitrogen to 10mL by using deionized water for later use; taking 1-3 mL of liquid essence, adding deionized water to a constant volume of 10mL for later use;
the fatty acid is any one of nonanoic acid, heptanoic acid and octanoic acid, the nonionic surfactant is TMN-6, and the ratio of the fatty acid to the nonionic surfactant is 5: 1;
the dosage of the ammonia water is 0.3-0.6 mL added in each 10mL of sample liquid;
the dosage of the hydrochloric acid is 1-2 mL added in each 10mL of sample liquid;
the magnetic Fe3O4The dosage of the nano particles is 5 ~ 10mg added in each 10mL of sample liquid;
the vortex time is 1 ~ 3 min;
the centrifugal rotating speed is 3000 ~ 5000r/min, and the time is 5 ~ 10 min;
the high performance liquid chromatography conditions are as follows: mobile phase: isocratic elution of methanol-water solution, methanol-water ratio of 65:35, detection wavelength: 296nm, column temperature: 25 ℃, flow rate: 1 mL/min.
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| CN110568103A (en) * | 2019-09-20 | 2019-12-13 | 浙江省食品药品检验研究院 | Deuterium-substituted marker and application thereof in detection of edible essence 3-acetyl-2, 5-dimethylthiophene |
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| CN104655775A (en) * | 2015-02-10 | 2015-05-27 | 广西中烟工业有限责任公司 | Method for measuring 3-acetyl-2, 5-dimethyl thiophene in edible flavor and fragrance |
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| CN101975808A (en) * | 2010-10-18 | 2011-02-16 | 上海市七宝中学 | Magnetic ferroferric oxide nano particle as well as preparation method and application thereof |
| CN104655775A (en) * | 2015-02-10 | 2015-05-27 | 广西中烟工业有限责任公司 | Method for measuring 3-acetyl-2, 5-dimethyl thiophene in edible flavor and fragrance |
| CN104655753A (en) * | 2015-02-10 | 2015-05-27 | 广西中烟工业有限责任公司 | Method for determining 3-acetyl-2, 5-thioxene in food additive |
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