CN113607716A - Detection method of illegal food additive - Google Patents
Detection method of illegal food additive Download PDFInfo
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- CN113607716A CN113607716A CN202110894896.2A CN202110894896A CN113607716A CN 113607716 A CN113607716 A CN 113607716A CN 202110894896 A CN202110894896 A CN 202110894896A CN 113607716 A CN113607716 A CN 113607716A
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- food additive
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
- G01N21/62—Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light
- G01N21/63—Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light optically excited
- G01N21/65—Raman scattering
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N1/00—Sampling; Preparing specimens for investigation
- G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
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Abstract
The invention provides a detection method of illegal food additives, which comprises the following steps: extracting the detected object, and centrifuging to obtain supernatant; treating the supernatant through a column to obtain a solution to be tested for later use; uniformly mixing a gold sol reagent, a solution to be detected and a coagulant, and then placing the mixture in a detection bin of a spectrometer for scanning detection to detect whether illegal food additives exist or not; the gold sol reagent is prepared from a chloroauric acid aqueous solution and a trisodium citrate aqueous solution. The detection method can realize the detection of Sudan red I, Sudan red II, Sudan red III, Sudan red IV and rhodamine B in the poultry eggs, is suitable for on-site rapid detection, and has the advantages of wide application range, simple operation and the like. Overcomes the defects of complex operation, large equipment volume and incapability of being used on site in the prior art.
Description
Technical Field
The invention relates to the technical field of detection of illegal food additives, in particular to a method for detecting Sudan red series and a Roche B in poultry eggs.
Background
The sudan red series dyes are a group of artificially synthesized lipophilic azo compounds with phenyl azo naphthol as a main group. Rhodamine is a fat-soluble industrial dye, and Sudan red series and rhodamine B dyes have potential carcinogenic, teratogenic and mutagenic effects, are currently attributed to illegal food additives by various countries, and are substance objects which are mainly monitored in foods in recent years. Because of their bright color and resistance to fading, they are often added to food as coloring agents by lawbreakers. There are still some lawless persons who, driven by the interest, add such dyes to the feed to feed poultry, resulting in so-called "red-yellow eggs".
The existing national standard detection method mainly adopts a high performance liquid chromatography and high performance liquid chromatography-mass spectrometry combined method, and the detection method is complex, the pretreatment is complex, more equipment is involved, and the required organic solvent is complex. The method has high requirements on operators, large detection cost and relatively long detection speed. Therefore, it is necessary to provide a further solution to the above problems.
Disclosure of Invention
The invention aims to provide a detection method of illegal food additives, which overcomes the defects in the prior art.
In order to achieve the above object, the present invention provides a method for detecting illegal food additives, which comprises the following steps:
extracting the detected object, and centrifuging to obtain supernatant;
treating the supernatant through a column to obtain a solution to be tested for later use;
uniformly mixing a gold sol reagent, a solution to be detected and a coagulant, and then placing the mixture in a detection bin of a spectrometer for scanning detection to detect whether illegal food additives exist or not;
the gold sol reagent is prepared from a chloroauric acid aqueous solution and a trisodium citrate aqueous solution.
As an improvement of the detection method of the illegal food additive of the present invention, the illegal food additive comprises: sudan red I, Sudan red II, Sudan red III, Sudan red IV and rhodamine B which are added into eggs and used as dyes.
As an improvement of the detection method of the illegal food additive, the step of extracting the detected object and obtaining the supernatant after centrifugation comprises the following steps:
providing 2g of detected object, adding 10 mL of extraction reagent, carrying out ultrasonic extraction for 10 minutes, centrifuging after extraction is finished, wherein the centrifugation speed is 10000 r/min, the centrifugation time is 2 minutes, and transferring 5mL of supernatant into a centrifuge tube after centrifugation.
As an improvement of the detection method of the illegal food additive, the extraction reagent is n-hexane.
As an improvement of the detection method of the illegal food additive, the step of processing the supernatant through a column to obtain a liquid to be tested for later use comprises the following steps:
adding 3mL of activating solution into an extraction column, adding 5mL of supernatant into the extraction column, performing column chromatography, adding 5mL of eluent, then adding 5mL of eluent for elution, drying the obtained eluent, redissolving the dried eluent by using 0.5mL of acetonitrile, and dissolving the redissolved eluent to be used as a liquid to be detected for later use.
As an improvement of the detection method of illegal food additives, the extraction column is a neutral alumina solid phase extraction column.
As an improvement of the detection method of illegal food additives, the activating solution and the leacheate are both normal hexane, and the eluent is 10% acetone-normal hexane.
As an improvement of the detection method of the illegal food additive, the step of uniformly mixing the gold sol reagent, the liquid to be detected and the coagulant and then placing the mixture in a detection bin of a spectrometer for scanning detection comprises the following steps:
and (3) taking 500 muL of gold sol reagent, 20 muL of liquid to be detected and 100uL of coagulant, uniformly mixing, and placing in a detection bin of a Raman spectrometer for scanning detection.
As an improvement of the detection method of the illegal food additive, the preparation method of the gold sol reagent comprises the following steps:
adding 100mL of ultrapure water into a 250mL three-neck round-bottom flask, quickly stirring and boiling, adding 1.2mL of 1% chloroauric acid aqueous solution, continuously heating to boil again, adding 1mL of 1% trisodium citrate aqueous solution, keeping stirring for about 25min, finishing the reaction, naturally cooling to room temperature, and sealing with a brown bottle for storage.
As an improvement of the detection method of illegal food additives, the coagulant is 0.2 mol/L sodium chloride solution.
Compared with the prior art, the invention has the beneficial effects that: the detection method can realize the detection of Sudan red I, Sudan red II, Sudan red III, Sudan red IV and rhodamine B in the poultry eggs, is suitable for on-site rapid detection, and has the advantages of wide application range, simple operation and the like. Overcomes the defects of complex operation, large equipment volume and incapability of being used on site in the prior art.
Drawings
In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings used in the description of the embodiments or the prior art will be briefly described below, it is obvious that the drawings in the following description are only some embodiments described in the present invention, and for those skilled in the art, other drawings can be obtained according to the drawings without creative efforts.
FIG. 1 is a standard spectrum of Sudan Red No. I obtained by the illegal food additive detection method of the present invention;
FIG. 2 is a standard spectrum of Sudan red No. II obtained by the illegal food additive detection method of the present invention;
FIG. 3 is a standard spectrum of Sudan red No. III obtained by the illegal food additive detection method of the present invention;
FIG. 4 is a standard spectrum of Sudan Red No. IV obtained by the illegal food additive detection method of the present invention;
FIG. 5 is a standard spectrum of rhodamine B obtained by the illegal food additive detection method of the present invention.
Detailed Description
The present invention is described in detail with reference to the following examples, but it should be understood that these examples are not intended to limit the present invention, and those skilled in the art should understand that the present invention is not limited to these examples, and functional, methodological, or structural equivalents and substitutions made by those skilled in the art are included in the scope of the present invention.
The invention provides a detection method of illegal food additives aiming at the detection of Sudan red series and a Roxist B in poultry eggs, which comprises the following steps:
extracting the detected object, and centrifuging to obtain supernatant;
treating the supernatant through a column to obtain a solution to be tested for later use;
uniformly mixing a gold sol reagent, a solution to be detected and a coagulant, and then placing the mixture in a detection bin of a spectrometer for scanning detection to detect whether illegal food additives exist or not;
the gold sol reagent is prepared from a chloroauric acid aqueous solution and a trisodium citrate aqueous solution.
Wherein the illegal food additive comprises: sudan red I, Sudan red II, Sudan red III, Sudan red IV and rhodamine B which are added into eggs and used as dyes. Therefore, the extraction and separation method is simple and easy to operate, and the spectrometer is small in size, so that the rapid field detection is facilitated.
The technical solution of the present invention will be described below by way of example with reference to an embodiment.
The illegal food additive detection method of the embodiment comprises the following steps:
and S1, extracting the detected object, and centrifuging to obtain a supernatant.
Specifically, step S1 includes: providing 2g of detected object, adding 10 mL of extraction reagent, carrying out ultrasonic extraction for 10 minutes, centrifuging after extraction is finished, wherein the centrifugation speed is 10000 r/min, the centrifugation time is 2 minutes, and transferring 5mL of supernatant into a centrifuge tube after centrifugation. Wherein the extraction reagent is n-hexane.
And S2, treating the supernatant through a column to obtain a liquid to be tested for later use.
Specifically, step S2 includes: adding 3mL of activating solution into an extraction column, adding 5mL of supernatant into the extraction column, performing column chromatography, adding 5mL of eluent, then adding 5mL of eluent for elution, drying the obtained eluent, redissolving the dried eluent by using 0.5mL of acetonitrile, and dissolving the redissolved eluent to be used as a liquid to be detected for later use. Wherein, the extraction column can be a neutral alumina solid phase extraction column. The activating solution and the eluent are both n-hexane, and the eluent can be 10% acetone-n-hexane.
S3, mixing gold sol reagent, solution to be detected and coagulant, placing the mixture in a spectrometer detection bin for scanning detection, and detecting whether illegal food additives exist.
Specifically, step S3 includes:
s31, preparing a gold sol reagent, wherein the preparation process comprises the following steps: adding 100mL of ultrapure water into a 250mL three-neck round-bottom flask, quickly stirring and boiling, adding 1.2mL of 1% chloroauric acid aqueous solution, continuously heating to boil again, adding 1mL of 1% trisodium citrate aqueous solution, keeping stirring for about 25min, finishing the reaction, naturally cooling to room temperature, and sealing with a brown bottle for storage. Wherein, the gold sol reagent is used for enhancing the signal of the detected substance so as to facilitate the subsequent spectrum detection.
S32, taking 500 muL of prepared gold sol reagent, 20 muL of solution to be detected and 100uL of coagulant, mixing uniformly, and placing in a detection bin of a Raman spectrometer for scanning detection. Wherein, the coagulant can be 0.2 mol/L sodium chloride solution. The standard spectrograms of Sudan red I, Sudan red II, Sudan red III, Sudan red IV and rhodamine B detected by a Raman spectrometer are shown in figures 1 to 5.
In conclusion, the detection method can realize the detection of Sudan red I, Sudan red II, Sudan red III, Sudan red IV and rhodamine B in the poultry eggs, is suitable for on-site rapid detection, and has the advantages of wide application range, simple operation and the like. Overcomes the defects of complex operation, large equipment volume and incapability of being used on site in the prior art.
It will be evident to those skilled in the art that the invention is not limited to the details of the foregoing illustrative embodiments, and that the present invention may be embodied in other specific forms without departing from the spirit or essential attributes thereof. The present embodiments are therefore to be considered in all respects as illustrative and not restrictive, the scope of the invention being indicated by the appended claims rather than by the foregoing description, and all changes which come within the meaning and range of equivalency of the claims are therefore intended to be embraced therein.
Furthermore, it should be understood that although the present description refers to embodiments, not every embodiment may contain only a single embodiment, and such description is for clarity only, and those skilled in the art should integrate the description, and the embodiments may be combined as appropriate to form other embodiments understood by those skilled in the art.
Claims (10)
1. The detection method of the illegal food additive is characterized by comprising the following steps:
extracting the detected object, and centrifuging to obtain supernatant;
treating the supernatant through a column to obtain a solution to be tested for later use;
uniformly mixing a gold sol reagent, a solution to be detected and a coagulant, and then placing the mixture in a detection bin of a spectrometer for scanning detection to detect whether illegal food additives exist or not;
the gold sol reagent is prepared from a chloroauric acid aqueous solution and a trisodium citrate aqueous solution.
2. The method for detecting illegal food additive according to claim 1, wherein the illegal food additive comprises: sudan red I, Sudan red II, Sudan red III, Sudan red IV and rhodamine B which are added into eggs and used as dyes.
3. The method for detecting illegal food additive according to claim 1 or 2, wherein the step of extracting the substance to be detected and centrifuging to obtain supernatant comprises:
providing 2g of detected object, adding 10 mL of extraction reagent, carrying out ultrasonic extraction for 10 minutes, centrifuging after extraction is finished, wherein the centrifugation speed is 10000 r/min, the centrifugation time is 2 minutes, and transferring 5mL of supernatant into a centrifuge tube after centrifugation.
4. The method for detecting illegal food additive according to claim 3, wherein the extracting reagent is n-hexane.
5. The method for detecting illegal food additive according to claim 1 or 2, wherein said "passing the supernatant through a column to obtain the liquid to be tested" comprises:
adding 3mL of activating solution into an extraction column, adding 5mL of supernatant into the extraction column, performing column chromatography, adding 5mL of eluent, then adding 5mL of eluent for elution, drying the obtained eluent, redissolving the dried eluent by using 0.5mL of acetonitrile, and dissolving the redissolved eluent to be used as a liquid to be detected for later use.
6. The method for detecting illegal food additive according to claim 5, wherein the extraction column is a neutral alumina solid phase extraction column.
7. The method for detecting illegal food additive according to claim 5, wherein the activating solution and the eluent are both n-hexane, and the eluent is 10% acetone-n-hexane.
8. The method for detecting the illegal food additive according to claim 1 or 2, wherein the step of uniformly mixing the gold sol reagent, the liquid to be detected and the coagulant and then placing the mixture in a spectrometer detection bin for scanning detection comprises the following steps:
and (3) taking 500 muL of gold sol reagent, 20 muL of liquid to be detected and 100uL of coagulant, uniformly mixing, and placing in a detection bin of a Raman spectrometer for scanning detection.
9. The method for detecting illegal food additive according to claim 8, wherein the preparation method of the gold sol reagent is as follows:
adding 100mL of ultrapure water into a 250mL three-neck round-bottom flask, quickly stirring and boiling, adding 1.2mL of 1% chloroauric acid aqueous solution, continuously heating to boil again, adding 1mL of 1% trisodium citrate aqueous solution, keeping stirring for about 25min, finishing the reaction, naturally cooling to room temperature, and sealing with a brown bottle for storage.
10. The method for detecting illegal food additive according to claim 1, wherein the coagulant is 0.2 mol/L NaCl solution.
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| CN202110894896.2A CN113607716A (en) | 2021-08-05 | 2021-08-05 | Detection method of illegal food additive |
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| CN202110894896.2A CN113607716A (en) | 2021-08-05 | 2021-08-05 | Detection method of illegal food additive |
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Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104034713A (en) * | 2013-03-05 | 2014-09-10 | 厦门大学 | Rapid detection method for Rhodamine B |
| CN111272913A (en) * | 2020-03-27 | 2020-06-12 | 石家庄学院 | Method for detecting sudan red residue in poultry eggs |
| CN111380858A (en) * | 2018-12-29 | 2020-07-07 | 同方威视技术股份有限公司 | Method for detecting Sudan red in food |
| CN113092445A (en) * | 2021-04-14 | 2021-07-09 | 中朗正健(苏州)生物技术有限公司 | Method for detecting illegal addition of omeprazole in weight-losing health-care food |
-
2021
- 2021-08-05 CN CN202110894896.2A patent/CN113607716A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104034713A (en) * | 2013-03-05 | 2014-09-10 | 厦门大学 | Rapid detection method for Rhodamine B |
| CN111380858A (en) * | 2018-12-29 | 2020-07-07 | 同方威视技术股份有限公司 | Method for detecting Sudan red in food |
| CN111272913A (en) * | 2020-03-27 | 2020-06-12 | 石家庄学院 | Method for detecting sudan red residue in poultry eggs |
| CN113092445A (en) * | 2021-04-14 | 2021-07-09 | 中朗正健(苏州)生物技术有限公司 | Method for detecting illegal addition of omeprazole in weight-losing health-care food |
Non-Patent Citations (1)
| Title |
|---|
| 林宏琳 等: "液-质联用法同时测定食品中罗丹明B和苏丹红染料", 中国卫生检验杂志, vol. 22, no. 10, pages 2302 - 2304 * |
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