CN111929401A - Quick authenticity identification evaluation method for pigeon soup based on GC-IMS analysis technology - Google Patents
Quick authenticity identification evaluation method for pigeon soup based on GC-IMS analysis technology Download PDFInfo
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- 235000014347 soups Nutrition 0.000 title claims abstract description 141
- 238000004458 analytical method Methods 0.000 title claims abstract description 26
- 238000005516 engineering process Methods 0.000 title claims abstract description 17
- 238000011156 evaluation Methods 0.000 title claims abstract description 14
- 238000000034 method Methods 0.000 claims abstract description 28
- 238000001514 detection method Methods 0.000 claims abstract description 20
- 238000010276 construction Methods 0.000 claims abstract description 14
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- 238000001228 spectrum Methods 0.000 claims description 15
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- AMQJEAYHLZJPGS-UHFFFAOYSA-N N-Pentanol Chemical compound CCCCCO AMQJEAYHLZJPGS-UHFFFAOYSA-N 0.000 description 4
- ZSIAUFGUXNUGDI-UHFFFAOYSA-N hexan-1-ol Chemical compound CCCCCCO ZSIAUFGUXNUGDI-UHFFFAOYSA-N 0.000 description 4
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- XEKOWRVHYACXOJ-UHFFFAOYSA-N Ethyl acetate Chemical compound CCOC(C)=O XEKOWRVHYACXOJ-UHFFFAOYSA-N 0.000 description 3
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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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Abstract
The invention relates to the technical field of pigeon soup identification, and particularly discloses a quick counterfeit identification evaluation method for pigeon soup based on a GC-IMS analysis technology. The quick identification and evaluation method for the pigeon soup based on the GC-IMS analysis technology comprises the following steps: and (3) standard feature map construction: the method comprises the following steps of (1) taking volatile components of the pigeon soup as detection objects, detecting the standard pigeon soup by adopting a gas phase-ion mobility spectrometer, and constructing a standard characteristic map of the standard pigeon soup based on the volatile components; constructing a characteristic map of the pigeon soup to be identified: detecting the pigeon soup to be identified by adopting the same gas phase-ion mobility spectrometer detection conditions as those in the standard characteristic map construction step to obtain a characteristic map of the pigeon soup to be identified based on volatile components; identifying the false pigeon soup: and comparing the characteristic map of the pigeon soup to be identified with the standard characteristic map, and judging the authenticity of the pigeon soup to be identified. The method can realize accurate and rapid identification of pigeon soup.
Description
Technical Field
The invention relates to the technical field of pigeon soup identification, in particular to a quick counterfeit identification evaluation method for pigeon soup based on a GC-IMS analysis technology.
Background
The pigeon soup is a soup stewed pigeon, is rich in nutrition, has certain health care effect, and can prevent and treat various diseases. The traditional Chinese medicine considers that the pigeon meat has the effects of tonifying liver and kidney, tonifying qi and blood, clearing away heat and toxic materials, promoting the production of body fluid and quenching thirst and the like.
Because of the above effects, pigeon soup is also gradually popularized in the market. However, with the popularization of pigeon soup, a lot of products which are fake with pigeon soup are continuously appeared. How to identify whether the pigeon soup is lack of modern detection means at present.
The gas phase-ion mobility spectrometer (GC-IMS) technology is a rapid and reliable analysis means for trace volatile organic gases, and has important application in the aspects of food, industry and environmental detection. At present, no report in the prior art adopts GC-IMS analysis technology to identify the authenticity of the pigeon soup.
Disclosure of Invention
The invention provides a quick counterfeit identification evaluation method for pigeon soup based on GC-IMS analysis technology, aiming at overcoming the technical defects of the prior art in the identification of the authenticity of the pigeon soup.
The technical scheme for solving the technical problems is as follows:
a pigeon soup rapid authenticity identification evaluation method based on GC-IMS analysis technology comprises the following steps:
and (3) standard feature map construction: the method comprises the following steps of (1) taking volatile components of the pigeon soup as detection objects, detecting the standard pigeon soup by adopting a gas phase-ion mobility spectrometer, and constructing a standard characteristic map of the standard pigeon soup based on the volatile components;
constructing a characteristic map of the pigeon soup to be identified: detecting the pigeon soup to be identified by adopting the same gas phase-ion mobility spectrometer detection conditions as those in the standard characteristic map construction step to obtain a characteristic map of the pigeon soup to be identified based on volatile components;
identifying the false pigeon soup: and comparing the characteristic map of the pigeon soup to be identified with the standard characteristic map, and judging the authenticity of the pigeon soup to be identified.
The method takes the volatile components of the pigeon soup as a detection object for the first time, and adopts a gas phase-ion mobility spectrometer to construct a standard characteristic map of the pigeon soup; then comparing the characteristic map of the pigeon soup to be identified with the standard characteristic map of the pigeon soup for identifying the authenticity of the pigeon soup; the method can rapidly and accurately identify the pigeon soup.
If the method is utilized in the specific implementation mode, the standard characteristic maps of the standard products of the pigeon soup of 18 days, the pigeon soup of 28 days and the old pigeon soup can be firstly constructed according to the method, then the characteristic map of the pigeon soup to be identified is detected according to the method, the characteristic map of the pigeon soup to be identified is compared with the standard characteristic map, and if the characteristic map of the pigeon soup to be identified is consistent with the standard characteristic map, the pigeon soup is obtained; if the characteristic map of the pigeon soup to be identified is not consistent with the standard characteristic map, the pigeon soup is not identified.
Further, the detection conditions of the gas phase-ion mobility spectrometer in the characteristic map construction step comprise: the chromatographic column is a capillary chromatographic column; the column temperature is 55-65 ℃; the carrier gas and the drift gas are nitrogen; the IMS temperature is 40-50 ℃; the analysis time is 25-35 min.
Further, the detection conditions of the gas phase-ion mobility spectrometer in the characteristic map construction step comprise: the chromatographic column is a capillary chromatographic column; the column temperature is 60 ℃; the carrier gas and the drift gas are nitrogen; the IMS temperature is 45 ℃; the analysis time was 25 min.
Furthermore, the chromatographic column is selected from a chromatographic column with the model number of FS-SE-54-CB-1.
Further, the sample pretreatment method of the pigeon soup before the sample injection by the gas phase-ion mobility spectrometer comprises the following steps: placing the pigeon soup in a headspace bottle, incubating at 75-85 ℃ for 15-25 min, and injecting a sample; most preferably, the pigeon soup is placed in a headspace bottle and injected after incubation at 80 ℃ for 20 min.
Further, the sample injection conditions of the gas phase-ion mobility spectrometer are as follows: the sample injection volume is 400-600 mu l; the temperature of the sample injection needle is 80-90 ℃.
Further, the sample injection conditions are as follows: the injection volume is 500 mul; the injection needle temperature was 85 ℃.
Further, gradient conditions of gas chromatography in the gas-ion mobility spectrometer are as follows:
at 0min, drift gas is 150ml/min, and carrier gas is 2 ml/min;
at 2min, drift gas is 150ml/min, and carrier gas is 2 ml/min;
when 10min, the drift gas is 150ml/min, and the carrier gas is 15 ml/min;
at 20min, drift gas is 150ml/min, and carrier gas is 80 ml/min;
at 25min, the drift gas is 150ml/min, and the carrier gas is 130 ml/min.
In the process of constructing the standard characteristic spectrum of the standard pigeon soup based on the volatile components of the pigeon soup by using the volatile components of the pigeon soup as detection objects and detecting the standard pigeon soup by using a gas phase-ion mobility spectrometer, the inventor further researches and discovers that the detection conditions of the gas phase-ion mobility spectrometer and the gradient conditions of gas chromatography play a critical role in determining whether a signal peak with higher separation degree can be obtained. The detection condition of the gas phase-ion mobility spectrometer and the gradient condition of the gas chromatography are not properly selected, the obtained signal peaks can be seriously overlapped, the obtained standard characteristic spectrum is difficult to distinguish, and the spectrum identification is difficult. The inventor finds that the signal peaks of the characteristic spectrum obtained under the detection condition of the gas phase-ion mobility spectrometer and the gradient condition of the gas chromatography have better separation degree, the standard spectrum of the pigeon soup is easy to distinguish, and the identification of the authenticity of the pigeon soup is convenient.
The sample pretreatment method plays a key role in enriching the volatile components of the pigeon soup, and a large number of experimental researches show that the inventor can enrich a large number of volatile components of the pigeon soup under the sample pretreatment method, so that the subsequent authenticity identification is facilitated.
Further, the characteristic spectrum is a GC-IMS fingerprint spectrum.
Further, the standard pigeon soup in the standard characteristic map construction step is 18-day pigeon soup, 28-day pigeon soup and old pigeon soup standard products.
Has the advantages that: the invention uses the volatile components of the pigeon soup as the detection object for the first time, and adopts a gas phase-ion mobility spectrometer to construct a characteristic map to identify the authenticity of the pigeon soup. In addition, the identification method can finish detection within 25min, and realize accurate and rapid identification of the authenticity of the pigeon soup.
Drawings
FIG. 1 shows standard gas chromatography-ion mobility spectrometry (GC-IMS) fingerprints of pigeon soup of different ages in days.
Figure 2 is a graph comparing standard gas chromatography-ion mobility spectrometry (GC-IMS) fingerprints of non-pigeon soup and pigeon soup.
In fig. 1 and 2, 18ri geling indicates pigeon soup of 18 days old, zishaguo indicates pigeon soup of 28 days old, laoge indicates old pigeon soup, jitang indicates chicken soup, and yatang indicates duck soup.
Detailed Description
The present invention will be further explained with reference to specific examples, which are not intended to limit the present invention in any way.
The gas chromatography-ion mobility spectrometer in the embodiment of the invention is specifically
A flavor analyzer;
the analysis software matched with the instrument comprises LAV (laboratory Analytical viewer) and three plugins as well as GC x IMS Library Search, and can be used for analyzing samples from different angles respectively.
And (5) LAV: used for checking and analyzing a spectrogram, wherein each point in the spectrogram represents a volatile organic compound; after a standard curve is established, quantitative analysis can be carried out.
Reporter plug-in: spectral differences between samples were directly compared (two-dimensional top view and three-dimensional spectra).
Gallery Plot insert: and the fingerprint spectra are compared, so that the difference of the volatile organic compounds among different samples is visually and quantitatively compared.
Dynamic PCA plug-in: and the dynamic principal component analysis is used for clustering and analyzing the samples and quickly determining the type of the unknown sample.
GC × IMS Library Search: the built-in NIST database and IMS database of application software can carry out qualitative analysis to the material, and the user can utilize the standard substance to expand the database by oneself according to the demand.
Example 1 Standard feature map construction method
Sample preparation: selecting pigeons 18 days old, pigeons 28 days old and old pigeons, putting the pigeons and the old pigeons into a purple clay pot, boiling the pigeons with strong fire, and stewing the pigeons with medium and small fire for 1.5 hours to obtain the pigeon soup.
Sample treatment: 1mL of pigeon soup is taken and placed in a 20mL headspace bottle, incubated at 80 ℃ for 20 minutes and injected. Each sample was injected 2 times in duplicate.
System conditions:
TABLE 1 analysis conditions
TABLE 2 gas chromatography conditions
| Time | E1 (drift gas) | E2 (Carrier gas) | R |
| 00:00,000 | 150mL/min | 2ml/min | Rec |
| 02:00,000 | 150mL/min | 2ml/min | - |
| 10:00,000 | 150mL/min | 15ml/min | - |
| 20:00,000 | 150mL/min | 80mL/min | - |
| 25:00,000 | 150mL/min | 130mL/min | Stop |
| 25:00,020 | 150mL/min | 130mL/min | --- |
Adopting the standard pigeon soup of different ages in days according to the above conditions
Analyzing by a flavor analyzer, and processing by the software to obtain standard gas chromatography-ion mobility spectrometry (GC-IMS) finger prints of pigeon soup with different ages in days as shown in figure 1.
The material in the right-most box of fig. 1 (red box) is a specific flavour in an 18-day pigeon soup, in much higher concentration than the other two pigeon soups; the bulk material in the second frame on the right (yellow frame) is specific flavor material in 28-day pigeon soup, including 1-butanol, ethanol, 1-hexanol, 1-propanol, 3-methylbutanal, 1-octen-3-one, acetoin, 1-octen-3-ol, 2-pentanone, ethyl acetate, 1-pentanol, 2, 3-butanedione, etc.; the material in the leftmost box (green box) is a specific flavour in pigeon soup. In addition, some substances, which are much higher in concentration than the old pigeon soup, are present in the pigeon soup of 18-day and 28-day pigeon ages, as shown in the third box (orange box) on the right side of fig. 1, including (E) -2-heptenal, 2-butanone, 2, 5-dimethylpyrazine, and the like.
As can be seen from FIG. 1, the standard map constructed by the method of the present invention can also clearly distinguish pigeon soup of different ages in days.
Example 2 fast identification and evaluation method of pigeon soup based on GC-IMS analysis technology
And (3) standard feature map construction: constructing standard characteristic spectrums (GC-IMS fingerprint spectrums) of 18-day-old pigeon soup, 28-day-old pigeon soup and old pigeon soup by taking the volatile components of the pigeon soup as detection objects according to the method in example 1;
constructing a characteristic map of the pigeon soup to be identified: referring to the method in example 1, obtaining a characteristic spectrum (GC-IMS fingerprint spectrum) of the pigeon soup to be identified;
identifying the false pigeon soup: and comparing the characteristic map of the pigeon soup to be identified with the standard characteristic map, and judging the authenticity of the pigeon soup to be identified. If the characteristic map of the pigeon soup to be identified is consistent with the standard characteristic map, the pigeon soup is identified; if the characteristic map of the pigeon soup to be identified is not consistent with the standard characteristic map, the pigeon soup is not identified.
In the embodiment, the pigeon soup to be identified is chicken soup and duck soup which are used for verifying the reliability of the method. In this example, the method for preparing the chicken soup and the duck soup was the same as that for preparing the pigeon soup in example 1.
As shown in FIG. 2, the substances in the rightmost frame (red frame) are specific volatile organic compounds in pigeon soup, including 1-pentanol, 2-butanone, 1-propanol, 1-octen-3-one, 3-methylbutanal, 1-butanol, acetoin, ethanol, 1-hexanol, 2, 3-butanedione, etc.; the material in the middle frame (yellow frame) is a specific volatile organic matter in the duck soup; in the leftmost box (orange box) are specific volatile organic compounds in chicken broth. The pigeon soup, the chicken soup and the duck soup can be clearly distinguished by the quick counterfeit identification evaluation method based on the GC-IMS analysis technology, and whether the pigeon soup to be identified is the pigeon soup can be accurately and clearly identified.
Claims (10)
1. A pigeon soup rapid authenticity identification evaluation method based on GC-IMS analysis technology is characterized by comprising the following steps:
and (3) standard feature map construction: the method comprises the following steps of (1) taking volatile components of the pigeon soup as detection objects, detecting the standard pigeon soup by adopting a gas phase-ion mobility spectrometer, and constructing a standard characteristic map of the standard pigeon soup based on the volatile components;
constructing a characteristic map of the pigeon soup to be identified: detecting the pigeon soup to be identified by adopting the same gas phase-ion mobility spectrometer detection conditions as those in the standard characteristic map construction step to obtain a characteristic map of the pigeon soup to be identified based on volatile components;
identifying the false pigeon soup: and comparing the characteristic map of the pigeon soup to be identified with the standard characteristic map, and judging the authenticity of the pigeon soup to be identified.
2. The method for fast appraising the authenticity of pigeon soup based on GC-IMS analysis technique as claimed in claim 1,
the detection conditions of the gas phase-ion mobility spectrometer in the characteristic map construction step comprise: the chromatographic column is a capillary chromatographic column; the column temperature is 55-65 ℃; the carrier gas and the drift gas are nitrogen; the IMS temperature is 40-50 ℃; the analysis time is 25-35 min.
3. The method for fast appraising the authenticity of pigeon soup based on GC-IMS analysis technique as claimed in claim 2,
the detection conditions of the gas phase-ion mobility spectrometer in the characteristic map construction step comprise: the chromatographic column is a capillary chromatographic column; the column temperature is 60 ℃; the carrier gas and the drift gas are nitrogen; the IMS temperature is 45 ℃; the analysis time was 25 min.
4. The method for fast counterfeit discrimination and evaluation of pigeon soup based on GC-IMS analysis technique as claimed in claim 2, wherein the type of the chromatographic column is FS-SE-54-CB-1.
5. The method for rapidly identifying and evaluating the pigeon soup based on the GC-IMS analysis technology as claimed in claim 1, wherein the sample pretreatment method of the pigeon soup before the injection of the gas phase-ion mobility spectrometer comprises: placing the pigeon soup in a headspace bottle, incubating at 75-85 ℃ for 15-25 min, and injecting a sample; most preferably, the pigeon soup is placed in a headspace bottle and injected after incubation at 80 ℃ for 20 min.
6. The method for rapidly identifying and evaluating the pigeon soup according to claim 1 based on the GC-IMS analysis technology, wherein the gas phase-ion mobility spectrometer is used under the following injection conditions: the sample injection volume is 400-600 mu l; the temperature of the sample injection needle is 80-90 ℃.
7. The quick authenticity identification evaluation method for pigeon soup based on GC-IMS analysis technology according to claim 1, characterized in that the sample injection conditions are as follows: the injection volume is 500 mul; the injection needle temperature was 85 ℃.
8. The method for fast appraising the authenticity of pigeon soup based on GC-IMS analysis technique as claimed in claim 1, wherein the gradient condition of the gas chromatography in the gas-ion mobility spectrometer is:
at 0min, drift gas is 150ml/min, and carrier gas is 2 ml/min;
at 2min, drift gas is 150ml/min, and carrier gas is 2 ml/min;
when 10min, the drift gas is 150ml/min, and the carrier gas is 15 ml/min;
at 20min, drift gas is 150ml/min, and carrier gas is 80 ml/min;
at 25min, the drift gas is 150ml/min, and the carrier gas is 130 ml/min.
9. The method for fast counterfeit identification and evaluation of pigeon soup based on GC-IMS analysis technology as claimed in claim 1, wherein the characteristic spectrum is GC-IMS fingerprint spectrum.
10. The method for fast counterfeit discrimination and evaluation of pigeon soup based on GC-IMS analysis technology as claimed in claim 1, wherein the standard pigeon soup of the standard characteristic map construction step is selected from 18-day pigeon soup, 28-day pigeon soup and old pigeon soup standard.
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