CN111929401A - Quick authenticity identification evaluation method for pigeon soup based on GC-IMS analysis technology - Google Patents

Abstract

The invention relates to the technical field of pigeon soup identification, and specifically discloses a rapid identification and evaluation method for pigeon soup based on GC-IMS analysis technology. The method for fast identification and evaluation of pigeon soup based on GC-IMS analysis technology, which comprises the following steps: a standard feature map construction step: taking the volatile components of pigeon soup as the detection object, and using gas-phase ion mobility spectrometer to detect standard pigeon soup, Constructing a standard feature map of standard pigeon soup based on volatile components; step of constructing a feature map of pigeon soup to be identified: using the same gas phase-ion mobility spectrometer detection conditions as in the standard feature map construction step to detect the pigeon soup to be identified, The characteristic map of the pigeon soup to be identified based on the volatile components is obtained; the step of authenticating the pigeon soup is to compare the characteristic map of the pigeon soup to be identified with the standard feature map to determine the authenticity of the pigeon soup to be identified. This method can realize accurate and rapid identification of the authenticity of pigeon soup.

Description

A rapid identification and evaluation method of pigeon soup based on GC-IMS analysis technology

technical field

The invention relates to the technical field of pigeon soup identification, in particular to a rapid identification and evaluation method for pigeon soup based on GC-IMS analysis technology.

Background technique

Pigeon is a kind of animal with great nutritional value. Pigeon soup is stewed soup for edible pigeons. Pigeon soup is not only nutritious, but also has certain health care effects, which can prevent and treat various diseases. Traditional Chinese medicine believes that pigeon meat has the functions of nourishing the liver and strengthening the kidney, nourishing qi and nourishing blood, clearing away heat and detoxifying, producing body fluid and quenching thirst.

Due to the above-mentioned effects of pigeon soup, pigeon soup has gradually become popular in the market. However, with the popularity of pigeon soup, many counterfeit pigeon soup products are also emerging. How to identify whether it is pigeon soup, there is currently a lack of modern detection methods.

Gas-Ion Mobility Spectrometry (GC-IMS) is a fast and reliable method for the analysis of trace volatile organic gases, and has important applications in food, industrial and environmental testing. There is also no prior art report using GC-IMS analysis technology to identify the authenticity of pigeon soup.

SUMMARY OF THE INVENTION

In order to overcome the above-mentioned technical defects in the authenticity identification of pigeon soup in the prior art, the present invention provides a rapid identification and evaluation method for pigeon soup based on GC-IMS analysis technology.

The technical scheme that the present invention solves the above-mentioned technical problems is as follows:

A kind of pigeon soup rapid identification and evaluation method based on GC-IMS analysis technology, it comprises the following steps:

Standard feature map construction step: take the volatile components of pigeon soup as the detection object, use gas-phase-ion mobility spectrometer to detect the standard pigeon soup, and construct a standard feature map of standard pigeon soup based on volatile components;

The step of constructing the characteristic map of the pigeon soup to be identified: the pigeon soup to be identified is detected using the same gas-phase-ion mobility spectrometer detection conditions as in the standard feature map construction step, and the characteristic map of the pigeon soup to be identified based on the volatile components is obtained;

The step of identifying the fake pigeon soup: comparing the feature map of the pigeon soup to be identified with the standard feature map to determine the authenticity of the pigeon soup to be identified.

The invention takes the volatile components of pigeon soup as the detection object for the first time, and uses gas-phase-ion mobility spectrometer to construct the standard characteristic map of pigeon soup; Identify the authenticity of pigeon soup; this method can quickly and accurately identify the authenticity of pigeon soup.

If the present invention is used in the specific embodiment, the standard feature map of the pigeon soup on the 18th, the pigeon soup on the 28th and the old pigeon soup can be constructed according to the above method, and then the pigeon soup to be identified is detected by the above method. Feature map, compare the feature map of pigeon soup to be identified with the standard feature map, if the feature map of pigeon soup to be identified is consistent with the standard feature map, it is pigeon soup; if the feature map of pigeon soup to be identified is inconsistent with the standard feature map , it is not pigeon soup.

Further, the detection conditions of the gas-ion mobility spectrometer in the feature map construction step include: the chromatographic column is a capillary chromatographic column; the column temperature is 55-65°C; the carrier gas and drift gas are nitrogen; the IMS temperature is 40-50°C; The time is 25 to 35 minutes.

Further, the detection conditions of the gas-ion mobility spectrometer in the feature map construction step include: the chromatographic column is a capillary chromatographic column; the column temperature is 60°C; the carrier gas and drift gas are nitrogen; the IMS temperature is 45°C; the analysis time is 25min .

Further, the described chromatographic column selects the chromatographic column whose model is FS-SE-54-CB-1.

Further, the sample pretreatment method of pigeon soup before sampling by gas-ion mobility spectrometer is as follows: placing pigeon soup in a headspace vial, incubating at 75-85° C. for 15-25 minutes, and then injecting the sample; Pigeon broth was placed in a headspace vial, incubated at 80 °C for 20 min and then injected.

Further, the sampling conditions of the gas phase-ion mobility spectrometer are: the sampling volume is 400-600 μl; the temperature of the sampling needle is 80-90°C.

Further, the injection conditions were as follows: the injection volume was 500 μl; the temperature of the injection needle was 85°C.

Further, the gradient conditions of the gas chromatography in the gas-ion mobility spectrometer are:

At 0min, the drift gas is 150ml/min and the carrier gas is 2ml/min;

At 2min, the drift gas is 150ml/min and the carrier gas is 2ml/min;

At 10min, the drift gas is 150ml/min and the carrier gas is 15ml/min;

At 20min, the drift gas is 150ml/min and the carrier gas is 80ml/min;

At 25min, the drift gas was 150ml/min and the carrier gas was 130ml/min.

Taking the volatile components of pigeon soup as the detection object, using gas-phase-ion mobility spectrometer to detect the standard pigeon soup, and constructing the standard characteristic map of the standard pigeon soup based on the volatile components of pigeon soup, the inventor further researched and found that the gas-phase- The detection conditions of ion mobility spectrometer and the gradient conditions of gas chromatography play a key role in obtaining signal peaks with higher resolution. If the detection conditions of gas-ion mobility spectrometer and the gradient conditions of gas chromatography are not properly selected, the obtained signal peaks have serious overlapping, and the obtained standard characteristic spectra are not easy to distinguish, which will make the identification of spectra difficult. The inventor found through a large number of studies that the signal peaks of the characteristic atlas obtained under the above-mentioned gas-ion mobility spectrometer detection conditions and the gradient conditions of the gas chromatography have a good degree of separation, and the standard atlas of pigeon soup is easy to distinguish, which is convenient for pigeon soup. Authenticity identification.

The sample pretreatment method plays a key role in whether the volatile components of pigeon soup can be enriched. The inventors have conducted a large number of experimental studies and have shown that a large number of volatile components of pigeon soup can be enriched under the above sample pretreatment method, which is convenient for Subsequent authentication.

Further, the characteristic spectrum is a GC-IMS fingerprint spectrum.

Further, the standard pigeon soup in the standard feature map construction step is selected from the 18th pigeon soup, the 28th pigeon soup and the old pigeon soup standard.

Beneficial effects: The present invention takes the volatile components of pigeon soup as the detection object for the first time, and uses gas-phase-ion mobility spectrometer to construct a characteristic map to identify the authenticity of pigeon soup. In addition, the identification method of the present invention can complete the detection within 25 minutes, thereby realizing accurate and rapid identification of the authenticity of pigeon soup.

Description of drawings

Figure 1 shows the standard gas chromatography-ion mobility spectrometry (GC-IMS) fingerprints of pigeon soup of different ages.

Figure 2 is a comparison diagram of the standard gas chromatography-ion mobility spectrometry (GC-IMS) fingerprints of the non-geozi soup and the pigeon soup.

In Figures 1 and 2, 18ri geling means 18-day-old pigeon soup, zishaguo means 28-day-old pigeon soup, laoge means old pigeon soup, jitang means chicken soup, and yatang means duck soup.

Detailed ways

The present invention is further explained below in conjunction with specific embodiments, but the embodiments do not limit the present invention in any form.

风味分析仪；The gas chromatography-ion mobility spectrometer in the embodiment of the present invention is specifically

flavor analyzer;

The analysis software provided with the instrument includes LAV (Laboratory Analytical Viewer), three plug-ins and GC×IMS Library Search, which can analyze samples from different angles.

LAV: used to view the analysis spectrum, each point in the graph represents a volatile organic compound; quantitative analysis can be performed after establishing a standard curve.

Reporter plugin: Directly compare spectral differences between samples (2D top view and 3D spectra).

Gallery Plot plug-in: Fingerprint comparison, intuitive and quantitative comparison of volatile organic compounds differences between different samples.

Dynamic PCA plug-in: dynamic principal component analysis, used to cluster samples and quickly determine the type of unknown samples.

GC×IMS Library Search: The built-in NIST database and IMS database of the application software can conduct qualitative analysis of substances, and users can expand the database by themselves using standard products according to their needs.

Embodiment 1 Standard feature map construction method

Sample preparation: Select 18-day-old pigeons, 28-day-old pigeons and old pigeons into a purple casserole pot, boil them on high heat first, and then simmer on medium and low heat for 1.5 hours to obtain pigeon soup.

Sample processing: Take 1 mL of pigeon soup, put it in a 20 mL headspace bottle, incubate at 80°C for 20 minutes and inject the sample. Each sample was injected 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 ---

风味分析仪进行分析，并采用上述软件处理得到图1为不同日龄鸽子汤的标准气相色谱-离子迁移谱(GC-IMS)指纹图谱。The pigeon soup standard products of different ages were adopted according to the above conditions

Flavor analyzer was used for analysis, and the above software was used to obtain the standard gas chromatography-ion mobility spectrometry (GC-IMS) fingerprints of pigeon soup of different ages.

The substances in the rightmost box (red box) in Figure 1 are the specific flavor substances in pigeon soup on the 18th, and its concentration is much higher than that of the other two kinds of pigeon soup; the second box on the right (yellow box) A large number of substances are specific flavor substances in pigeon soup on the 28th, 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 and 2,3-butanedione, etc.; the substance in the leftmost box (green box) is pigeon soup specific flavor substances in . In addition, there are some substances in the pigeon soup at the age of 18 and 28 that are much higher than that of the old pigeon soup, as shown in the third box (orange box) on the right side of Figure 1, including (E)-2-heptene Aldehyde, 2-butanone and 2,5-dimethylpyrazine, etc.

As can be seen from Figure 1, the standard map constructed by the method of the present invention can also clearly distinguish pigeon soup of different ages.

Example 2 Rapid identification and evaluation method of pigeon soup based on GC-IMS analysis technology

Standard feature map construction step: take the volatile components of pigeon soup as the detection object, with reference to the method of Example 1, construct standard feature maps (GC-IMS fingerprints) of 18-day-old pigeon soup, 28-day-old pigeon soup and Laoge soup ;

To-be-identified pigeon soup feature atlas construction step: refer to the method of embodiment 1 with pigeon-to-be-identified soup, obtain the characteristic atlas (GC-IMS fingerprint spectrum) of pigeon soup to be identified;

The step of identifying the fake pigeon soup: comparing the feature map of the pigeon soup to be identified with the standard feature map to determine the authenticity of the pigeon soup to be identified. If the feature map of pigeon soup to be identified is consistent with the standard feature map, it is pigeon soup; if the feature map of pigeon soup to be identified is inconsistent with the standard feature map, it is not pigeon soup.

In this embodiment, the pigeon soup to be identified uses chicken soup and duck soup to verify the reliability of the method of the present invention. For the preparation methods of chicken soup and duck soup in this example, refer to the preparation method of pigeon soup in Example 1.

The results are shown in Figure 2. The substances in the far right box (red box) are specific volatile organic compounds in pigeon soup, including 1-pentanol, 2-butanone, 1-propanol, and 1-octene-3 - ketone, 3-methylbutanal, 1-butanol, acetoin, ethanol, 1-hexanol and 2,3-butanedione, etc.; the substances in the middle box (yellow box) are specific in duck soup Volatile organic compounds; the leftmost box (orange box) is the specific volatile organic compounds in chicken broth. This shows that the pigeon soup, chicken soup and duck soup can be clearly distinguished by the pigeon soup rapid identification and evaluation method based on the GC-IMS analysis technology of the present invention, and whether the pigeon soup to be identified is pigeon soup can be accurately and clearly identified.

Claims (10)

1. a kind of pigeon soup based on GC-IMS analysis technique is characterized in that, it is characterized in that, comprises the steps: Standard feature map construction step: take the volatile components of pigeon soup as the detection object, use gas-phase-ion mobility spectrometer to detect the standard pigeon soup, and construct a standard feature map of standard pigeon soup based on volatile components; The step of constructing the characteristic map of the pigeon soup to be identified: the pigeon soup to be identified is detected using the same gas-phase-ion mobility spectrometer detection conditions as in the standard feature map construction step, and the characteristic map of the pigeon soup to be identified based on the volatile components is obtained; The step of identifying the fake pigeon soup: comparing the feature map of the pigeon soup to be identified with the standard feature map to determine the authenticity of the pigeon soup to be identified. 2. the pigeon soup quick identification and evaluation method based on GC-IMS analysis technology according to claim 1 is characterized in that, The detection conditions of the gas-ion mobility spectrometer in the characteristic map construction step include: the chromatographic column is a capillary chromatographic column; the column temperature is 55-65° C.; the carrier gas and the drift gas are nitrogen; the IMS temperature is 40-50° C.; the analysis time is 25 ~35min. 3. the pigeon soup quick identification and evaluation method based on GC-IMS analysis technology according to claim 2 is characterized in that, The detection conditions of gas-ion mobility spectrometer in the characteristic map construction step include: the chromatographic column is a capillary column; the column temperature is 60°C; the carrier gas and drift gas are nitrogen; the IMS temperature is 45°C; and the analysis time is 25min. 4. the pigeon soup quick identification and evaluation method based on GC-IMS analysis technology according to claim 2, is characterized in that, described chromatographic column selection model is the chromatographic column of FS-SE-54-CB-1. 5. the pigeon soup fast identification and evaluation method based on GC-IMS analysis technology according to claim 1, is characterized in that, the sample pretreatment method of pigeon soup before gas-phase-ion mobility spectrometer sample introduction is: by pigeon soup Place in a headspace vial, incubate at 75-85°C for 15-25min, and inject; most preferably, place pigeon soup in a headspace vial, incubate at 80°C for 20min, and inject. 6. The pigeon soup rapid identification and evaluation method based on GC-IMS analysis technology according to claim 1, wherein the sampling conditions of the gas-phase-ion mobility spectrometer are: the sampling volume is 400-600 μl; The needle temperature is 80 to 90°C. 7 . The pigeon soup rapid identification and evaluation method based on GC-IMS analysis technology according to claim 1 , wherein the sample injection conditions are: the sample injection volume is 500 μl; the injection needle temperature is 85° C. 8 . 8. the pigeon soup quick identification and evaluation method based on GC-IMS analysis technology according to claim 1, is characterized in that, the gradient condition of gas chromatography in gas-ion mobility spectrometer is: At 0min, the drift gas is 150ml/min and the carrier gas is 2ml/min; At 2min, the drift gas is 150ml/min, and the carrier gas is 2ml/min; At 10min, the drift gas is 150ml/min and the carrier gas is 15ml/min; At 20min, the drift gas is 150ml/min and the carrier gas is 80ml/min; At 25min, the drift gas was 150ml/min and the carrier gas was 130ml/min. 9. The pigeon soup quick identification and evaluation method based on GC-IMS analysis technology according to claim 1, is characterized in that, described characteristic spectrum is GC-IMS fingerprint spectrum. 10. the pigeon soup fast identification and evaluation method based on GC-IMS analysis technology according to claim 1, is characterized in that, the standard pigeon soup of standard feature map construction step selects 18th pigeon old pigeon soup, 28th pigeon old pigeon soup Soup and old pigeon soup standard.

Images