CN115290804A - Fingerprint spectrum of allspice extract for food and construction method thereof - Google Patents

Fingerprint spectrum of allspice extract for food and construction method thereof Download PDF

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CN115290804A
CN115290804A CN202210989671.XA CN202210989671A CN115290804A CN 115290804 A CN115290804 A CN 115290804A CN 202210989671 A CN202210989671 A CN 202210989671A CN 115290804 A CN115290804 A CN 115290804A
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extract
allspice
fingerprint
flavor
food
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刘娜
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Tianjin Chunfa Bio Technology Group Co Ltd
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Tianjin Chunfa Bio Technology Group Co Ltd
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    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N30/00Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
    • G01N30/02Column chromatography
    • G01N30/04Preparation or injection of sample to be analysed
    • G01N30/06Preparation
    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N30/00Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
    • G01N30/02Column chromatography
    • G01N30/62Detectors specially adapted therefor
    • G01N30/72Mass spectrometers
    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N30/00Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
    • G01N30/02Column chromatography
    • G01N30/86Signal analysis
    • G01N30/8675Evaluation, i.e. decoding of the signal into analytical information
    • G01N30/8686Fingerprinting, e.g. without prior knowledge of the sample components
    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N33/00Investigating or analysing materials by specific methods not covered by groups G01N1/00 - G01N31/00
    • G01N33/0001Investigating or analysing materials by specific methods not covered by groups G01N1/00 - G01N31/00 by organoleptic means

Abstract

The invention relates to a finger print of a passion fruit extract for food and a construction method thereof. The preparation method of the allspice extract for food has the advantages of high extraction efficiency, small flavor loss, effective retention of flavor components and the like.

Description

Fingerprint spectrum of allspice extract for food and construction method thereof
Technical Field
The invention relates to the technical field of food, in particular to a preparation method of a allspice extract for food, a fingerprint of the prepared allspice extract and a construction method of the allspice extract.
Background
The allspice, also known as jamaica pepper, three spices sweet pepper, etc., is a natural antioxidant, is native to west indian islands and middle beauty, and is called allspice because it has a mixed aromatic odor similar to clove, cinnamon and nutmeg.
The allspice is mainly prepared from dry seeds of allspice, contains abundant volatile oil, is a spice containing polyphenol substances, and mainly comprises eugenol, methyl eugenol, protein, fat, vitamin A, vitamin C, vitamin B1, vitamin B2 and various minerals. The allspice can be used in tobacco, cosmetic, food, etc., and has antibacterial, antiinflammatory, insect preventing, and antioxidant effects.
The fingerprint refers to a technology that the product identity can be analyzed and identified after specific quality (such as aroma, element composition, color and the like) of a substance is subjected to specific informatization processing, and the identification has uniqueness and can be used for identifying the authenticity of the product and judging the quality of the product.
However, the related art has less research on the allspice and less research on the allspice for food.
Disclosure of Invention
The present invention is based on the discovery and recognition by the inventors of the following facts and problems: at present, the method mainly adopts an aqueous solvent extraction method, an ethyl acetate extraction method and the like, and because the main volatile components of the allspice, such as eugenol and the like, have low solubility in water, the aqueous solvent extraction method has low extraction rate and great loss of flavor substances; the ethyl acetate extraction preparation method improves the extraction rate, and has good effect when being applied to the tobacco industry. However, in the food industry, ethyl acetate flavor can affect the overall flavor of the extract, thereby affecting food flavor. Meanwhile, the research and report of the fingerprint spectrum of the flavor substances are hardly seen.
In view of the above, the present invention aims to provide a preparation method of a allspice extract for food, and simultaneously establish a characteristic flavor substance analysis method and a fingerprint spectrum thereof, so as to provide a theoretical basis for allspice flavor research and development and utilization thereof, better develop related flavor products, and effectively promote the development of the food industry.
Therefore, the embodiment of the invention provides a method for constructing a fingerprint spectrum of a food-grade allspice extract, which comprises the following steps:
(1) Preparation of Pimenta dioica extract
Cleaning allspice, drying in 40 deg.C oven for 2 hr, crushing, and sieving with 100 mesh sieve; then adding 20-30% ethanol water solution according to the mass ratio of 1 (20-30), soaking for 2-3h, and performing ultrasonic extraction for 90-120min; centrifuging the material after ultrasonic treatment, and collecting filtrate; ethanol was removed rapidly using a rotary evaporator; concentrating at low temperature to 1/5 of the original volume to obtain Pimenta dioica extract;
(2) Method for extracting flavor substance
Placing the allspice extract obtained in the step (1) in a headspace bottle, sealing and capping, placing in a thermostat, and balancing for 20min at 60 ℃;
(3) Solid phase microextraction-gas chromatography-mass spectrometry combination
Inserting a solid phase microextraction extraction head into the headspace bottle in the step (2), performing headspace extraction at 60 ℃ for 45min, taking out the extraction head, immediately inserting into a Gas Chromatography (GC) sample inlet, desorbing for 5min, and performing sample injection analysis;
gas chromatography conditions: hp-5 capillary column (30 m × 0.25mm × 0.25 μm), injection inlet temperature 250 deg.C, carrier gas of high-purity helium gas greater than or equal to 99.999%, carrier gas flow rate of 1.0mL/min, temperature programming: the initial temperature is 40 ℃, the temperature is kept for 2.0min, the temperature is increased to 150 ℃ at 3 ℃/min, and then the temperature is increased to 230 ℃ at 10 ℃/min, and the temperature is kept for 10.0min;
mass spectrum conditions: an EI ion source; electron energy 70eV; the temperature of the four-level bar is 150 ℃, and the interface temperature is 250 ℃; electron multiplier voltage 1075V; the ion source temperature is 230 ℃; tuning in a standard manner; selecting a full SCAN (SCAN) mode, wherein the mass SCAN range is as follows: 35 to 450amu.
In some embodiments, the preparing the pimenta dioica extract comprises the steps of: cleaning allspice, drying in 40 deg.C oven for 2 hr, crushing, and sieving with 100 mesh sieve; then adding 20% ethanol water solution according to the mass ratio of 1; centrifuging the material after ultrasonic treatment, and collecting filtrate; ethanol was removed rapidly using a rotary evaporator; concentrating at low temperature to 1/5 of the original volume to obtain Pimenta dioica extract.
In some embodiments, 2-3g of the allspice extract from step (2) is placed in a 20mL headspace bottle.
In some embodiments, the solid phase microextraction extraction head is polyethylene glycol-polydimethylsiloxane (CAR/PDMS) with a coating thickness of 100 μm. Available directly from commercial sources, such as Supelco, USA.
In some embodiments, the solid phase micro extraction head is subjected to an aging treatment at 250 ℃ for 30min before the head space extraction.
In some embodiments, the method for constructing a fingerprint further includes: the gas chromatography and the smell are combined, a shunt port is arranged at the tail end of a gas chromatography column to shunt 1 part of the capillary column, one part is connected with a mass spectrum detector to perform mass spectrum identification, the other part is connected with an odor detector to identify the flavor characteristics of the single component through human olfaction.
In some embodiments, the method for constructing a fingerprint further includes: the Retention Index (RI) determination method comprises the steps of injecting C8-C40 normal alkane under the same analysis condition of gas chromatography-mass spectrometry, and calculating the RI value of a compound corresponding to a sample according to the retention time of the normal alkane.
In some embodiments, the method for constructing a fingerprint further includes: the key flavor compound method is established, under the analysis condition of gas chromatography-mass spectrometry, the contribution of each flavor component to the overall flavor of a sample is evaluated by using a Relative Odor Activity Value (ROAV), the ROAV value of the maximum flavor contribution component of the sample is set as 100, and the ROAV calculation formula of each compound is as follows:
ROAVi≈100×Ci/Cstan×Tstan/Ti
in the formula: ROAV i Is the relative odor activity value of a certain volatile flavor substance; c i Is the relative content of certain volatile flavor substances; t is stan A threshold value that contributes the most volatile flavour substances to the odour; c stan The relative amount of the most volatile flavor that contributes to the odor; t is a unit of i Is the olfactive threshold of a certain volatile component.
When ROAV is more than or equal to l, the compound is the characteristic flavor component of the allspice extract.
The embodiment of the invention also provides a fingerprint spectrum of the food passion fruit extract constructed by the method.
In some embodiments, the fingerprint of the Pimenta dioica extract has 15 common characteristic peaks, and the relative retention times of the common characteristic peaks are respectively as follows: 12.927, 14.594, 15.505, 17.993, 21.554, 22.213, 25.249, 26.550, 30.617, 31.153, 32.472, 32.703, 33.890, 36.606 and 41.674min, which are taken as the standard fingerprint of the allspice extract for food.
In some embodiments, the standard fingerprint of the allspice extract has 6 characteristic flavor component peaks, and the relative retention times of the characteristic flavor component peaks are respectively: 30.617, 32.703, 32.472, 14.594, 12.927 and 17.993min.
The invention has the advantages and beneficial effects that:
(1) The method for constructing the passion fruit extract fingerprint spectrum can comprehensively and accurately reflect the aroma quality condition of a sample, can monitor the quality of different batches of the passion fruit, is simple, has strong operability, and provides a quick, effective and simple method for quality evaluation.
(2) The preparation method of the allspice extract for food, provided by the invention, has the advantages of higher extraction efficiency, small flavor loss, effective retention of flavor components and the like.
(3) The invention adopts a solid phase microextraction method to collect flavor substances aiming at the allspice extract, utilizes a gas chromatography-mass spectrometry combined method to analyze volatile components, further preferably combines the gas chromatography-smelling combined method, retention indexes, odor activity values (ROAV) and the like to evaluate and analyze the flavor substances, and obtains the characteristic flavor substance composition of the allspice extract, and the method is accurate and has high accuracy.
(3) The fingerprint of the allspice extract constructed by the invention provides a theoretical basis for researching and developing the allspice flavor, better develops related flavor products and effectively promotes the development of the food industry.
Drawings
Fig. 1 is a total ion flow diagram of flavor analysis of a pimento extract. Figures 1-24 correspond to the numbering in table 5.
Detailed Description
The embodiments of the present invention will be described in detail below, and the embodiments described below by referring to the drawings are exemplary and intended to be used for explaining the present invention, and should not be construed as limiting the present invention.
Example 1
The preparation method of the food passion fruit extract comprises the following steps:
cleaning allspice, drying in oven at 40 deg.C for 2 hr, crushing with food processor, repeating for 3 times, and sieving with 100 mesh sieve; then adding 20% ethanol water solution according to the mass ratio of 1; centrifuging the material after ultrasonic treatment, and collecting filtrate; ethanol was removed rapidly using a rotary evaporator; concentrating at low temperature (low temperature concentration at 10 deg.C by using low temperature condensing device) to 1/5 of the original volume to obtain Pimenta dioica extract.
The parameters of the method steps in example 1, including the mass ratio of the material to the extraction solvent, the ethanol content in the extraction solvent, the soaking time and the extraction time, were changed, and the results are shown in tables 1 to 4, taking into account the influence of the parameter changes on the normalized content of the eugenol peak area in the flavor measurement.
Influence factor investigation experiment: the mass ratio of the materials to the extraction solvent, the content of ethanol in the extractant, the soaking time and the extraction time are mainly considered to influence the peak area normalized content of the eugenol in the flavor substance determination, and the optimal extraction condition factor level is determined.
TABLE 1 level investigation of the mass ratio of materials and extraction solvent
Figure BDA0003803382720000041
As can be seen from table 1, the peak area content of eugenol gradually increases with the increase of the extraction solvent, and when the mass ratio of the material to the extraction solvent is 1.
TABLE 2 level investigation experiment of ethanol content in extractant
Figure BDA0003803382720000042
Figure BDA0003803382720000051
As can be seen from table 2, the peak area content of eugenol gradually increases with the increase of the ethanol content in the extraction solvent, and when the ethanol content is 20%, the ethanol content in the extraction solvent is increased, the peak area content of eugenol tends to be stable, and the ethanol content in the extraction solvent is determined to be 20% in consideration of the production cost.
Table 3 horizontal investigation experiment of soaking time
Figure BDA0003803382720000052
As can be seen from Table 3, the peak area content of eugenol gradually increases with the increase of the soaking time, when the soaking time is 2 hours, the soaking time is prolonged, the peak area content of eugenol slightly increases, and the soaking time is determined to be 2 hours in consideration of the length of the production process.
TABLE 4 horizontal examination of extraction time
Figure BDA0003803382720000053
As can be seen from Table 4, the peak area content of eugenol gradually increased with the increase of the extraction time, when the extraction time was 90min, the extraction time was increased again, the peak area content of eugenol slightly increased, when the extraction time was increased to 180min, the peak area content of eugenol slightly decreased, and the extraction time was determined to be 90min in consideration of the length of the production process.
Example 2
A method for constructing a finger print of a passion fruit extract for food comprises the following steps:
A. preparation method of food-grade allspice extract
Cleaning the allspice, placing in a drying oven, and drying at 40 ℃ for 2h; rapidly stirring into powder by using a food processor, repeating for 3 times, and sieving with a 100-mesh sieve; adding 20% ethanol water solution according to the mass ratio of 1; centrifuging the material after ultrasonic treatment, and collecting filtrate; ethanol was removed rapidly using a rotary evaporator; concentrating at 10 deg.C to 1/5 of the original volume to obtain high-quality allspice extract product.
B. Method for extracting flavor substance
Placing 2-3g of Pimenta dioica extract sample in 20mL headspace bottle, sealing and capping, placing in thermostat, and balancing at 60 deg.C for 20min.
C. The flavor substance identification method comprises the following steps: solid phase microextraction-gas chromatography-mass spectrometry combination
Solid phase micro-extraction device handle and 100um polyethylene glycol-polydimethylsiloxane (CAR/PDMS) extraction fiber head US Supelco
Solid phase micro-extraction: and (3) inserting the solid-phase micro-extraction device subjected to advanced aging treatment into a sealed bottle through a rubber gasket, pushing out an extraction head, performing headspace extraction for 45min, taking out the extraction head, immediately inserting into a GC sample inlet, desorbing for 5min, and performing sample injection analysis.
Gas chromatography conditions: hp-5 capillary column (30 m × 0.25mm × 0.25 μm), injection inlet temperature 250 deg.C, carrier gas is high-purity (greater than or equal to 99.999%) helium, carrier gas flow rate is 1.0mL/min, temperature programming: the initial temperature was 40 deg.C, held for 2.0min,3 deg.C/min raised to 150 deg.C, then raised to 230 deg.C at 10 deg.C/min, held for 10.0min.
Mass spectrum conditions: an EI ion source; electron energy 70eV; the temperature of the four-level bar is 150 ℃, and the interface temperature is 250 ℃; electron multiplier voltage 1075V; the ion source temperature is 230 ℃; tuning in a standard manner; selecting a full SCAN (SCAN) mode, wherein the mass SCAN range is as follows: 35 to 450amu.
D. Flavor substance identification results
The flavor analysis results are detailed in table 5, and the total ion flow analysis is shown in fig. 1.
TABLE 5 flavor analysis results
Figure BDA0003803382720000061
Figure BDA0003803382720000071
The substances may be non-fragrant or very slightly fragrant due to the high concentration of substances indicated in the chromatogram obtained by the MS detector. Therefore, the chromatogram obtained by using only MS detection does not show the aroma profile of the substance well. The human nose is a detector with high selectivity and high sensitivity, and is a good detector when detecting aromaticity. Can make up for the deficiency of the MS detector. Thus, in some embodiments, the process also performs gas phase sniffing. The smelling condition is that a shunting port is arranged at the tail end of a gas chromatographic column to shunt 1 part of the outlet of a capillary column, one part is connected with a mass spectrum detector to carry out mass spectrum identification, the other part is connected with an odor detector to identify the flavor characteristics of single components through human olfaction, the material flavor characteristics are detailed in a table 5, and the chromatographic retention time of the single component for two kinds of detection is basically consistent.
In addition, the step C can further comprise a retention index measuring method, wherein the normal paraffin of C8-C40 is injected under the same analysis condition of gas chromatography-mass spectrometry, and the RI value of the compound corresponding to the sample is calculated according to the retention time. The compound retention index RI is calculated as:
RI sample =100n + (Rt sample-Rtn) × 100/(Rtn + 1-Rtn)
Wherein, RI sample-RI of sample chromatographic peak; the Rt sample, the Rtn and the Rtn + 1-are respectively the retention time of a chromatographic peak of the sample and the retention time of a chromatographic peak of normal paraffin before and after the chromatographic peak of the sample flows out; n-the number of carbon atoms contained in the normal alkane before the chromatographic peak of the sample flows out.
In addition, the step C also includes establishing a key flavor compound method, evaluating the contribution of each flavor component to the overall flavor of the sample by using a Relative Odor Activity Value (ROAV) under the same analysis condition of gas chromatography-mass spectrometry, setting the ROAV value of the maximum flavor contribution component of the sample as 100, and calculating the ROAV of each compound according to the following formula:
ROAVi≈100×Ci/Cstan×Tstan/Ti
in the formula: ROAV i Is the relative odor activity value of a certain volatile flavor substance; c i Is the relative content of certain volatile flavor substances; t is a unit of stan Contribute to the smellA threshold of maximum volatile flavor; c stan The relative amount of the most volatile flavor that contributes to the odor; t is i Is the olfactive threshold of a volatile component; when ROAV is more than or equal to l, the compound is the characteristic flavor component of the allspice.
Through analysis, the relative content of the eugenol in the pimenta dioica flavor substance is high, the olfactory threshold is small, and therefore the eugenol has an important contribution to the flavor of the pimenta dioica extract, and the ROAV value of the eugenol in the pimenta dioica extract is defined as 100. The sensory threshold of each substance is obtained through inquiry, and the ROAV value of each substance is calculated according to an ROAV calculation formula and is shown in table 5 in detail.
D. Determination of standard fingerprint
Because the flavor of the allspice in different producing areas is different, the flavor substance analysis is carried out on 13 batches of samples of a certain allspice, 24 common peaks are determined, and the retention time is respectively as follows: 12.927, 14.294, 14.594, 15.525, 17.330, 17.993, 20.690, 21.554, 22.213, 22.340, 25.249, 26.550, 28.100, 30.617, 31.153, 32.472, 32.703, 33.890, 35.461, 36.606, 38.924, 39.680, 39.840 and 41.674min. The common characteristic peaks form the fingerprint characteristics of the extract of the allspice and can be used as the standard fingerprint spectrum of the allspice.
The flavor substance analysis is carried out on 13 commercially available allspice samples, 15 common characteristic peaks are determined, and the retention time is as follows: 12.927, 14.594, 15.525, 17.993, 21.554, 22.213, 25.249, 26.550, 30.617, 31.153, 32.472, 32.703, 33.890, 36.606 and 41.674min. The common characteristic peaks form the fingerprint characteristics of the allspice extract and can be used as the standard fingerprint spectrum of the allspice extract.
E. Determination of characteristic flavor component peaks of standard fingerprint spectrum
Through the calculation of relative odor activity values, the six substances of eugenol, caryophyllene, methyl eugenol, eucalyptol, beta-myrcene and linalool are characteristic flavor components of the allspice, so that component peaks of the six substances can be used as main spectrum peaks. Namely 30.617, 32.703, 32.472, 14.594, 12.927 and 17.993min, as characteristic flavor component peaks of the standard fingerprint spectrum of the allspice extract.
F. Method investigation
And (3) precision test:
taking a passion fruit sample, continuously measuring and analyzing for 6 times according to the preparation method of the passion fruit extract and the flavor substance identification method, recording a total ion flow diagram, and calculating the relative peak area and the relative retention time of each common peak by taking eugenol as a reference peak. RSD for each common peak relative peak area and relative retention time was less than 1.00% (n = 6), indicating good precision of the instrument.
And (3) stability test:
taking a allspice sample, respectively placing the allspice sample for 0, 2, 4, 8, 12, 18, 20 and 24 hours at room temperature (20-30 ℃) according to the preparation method of the allspice extract and the identification method of flavor substances, determining and analyzing, recording a total ion flow diagram, and calculating the relative peak area and the relative retention time of each common peak by taking eugenol as a reference peak. RSD for each common peak relative peak area and relative retention time was less than 3.00% (n = 8), indicating that the samples were stable well at room temperature for 24 h.
And (3) repeatability test:
taking a allspice sample, preparing 6 samples in parallel according to the preparation method of the allspice extract and the flavor substance identification method, measuring and analyzing, recording a total ion flow diagram, and calculating the relative peak area and the relative retention time of each common peak by taking eugenol as a reference peak. RSD for each common peak relative peak area and relative retention time was less than 5.00% (n = 6), indicating good reproducibility of the method.
In the present disclosure, the terms "one embodiment," "some embodiments," "an example," "a specific example," or "some examples" and the like mean that a specific feature, structure, material, or characteristic described in connection with the embodiment or example is included in at least one embodiment or example of the present disclosure. In this specification, the schematic representations of the terms used above are not necessarily intended to refer to the same embodiment or example. Furthermore, the particular features, structures, materials, or characteristics described may be combined in any suitable manner in any one or more embodiments or examples. Furthermore, various embodiments or examples and features of different embodiments or examples described in this specification can be combined and combined by one skilled in the art without contradiction.
Although embodiments of the present invention have been shown and described above, it is understood that the above embodiments are exemplary and should not be construed as limiting the present invention, and that variations, modifications, substitutions and alterations can be made to the above embodiments by those of ordinary skill in the art within the scope of the present invention.

Claims (10)

1. A construction method of a fingerprint of a allspice extract for food is characterized by comprising the following steps:
(1) Preparation of Pimenta dioica extract
Cleaning allspice, drying in 40 deg.C oven for 2 hr, crushing, and sieving with 100 mesh sieve; then adding 20-30% ethanol water solution according to the mass ratio of 1 (20-30), soaking for 2-3h, and performing ultrasonic extraction for 90-120min; centrifuging the material after ultrasonic treatment, and collecting filtrate; ethanol was removed rapidly using a rotary evaporator; concentrating at low temperature to 1/5 of the original volume to obtain Pimenta dioica extract;
(2) Method for extracting flavor substance
Placing the allspice extract obtained in the step (1) in a headspace bottle, sealing and capping, placing in a thermostat, and balancing for 20min at 60 ℃;
(3) Solid phase microextraction-gas chromatography-mass spectrometry combination
Inserting a solid phase microextraction extraction head into the headspace bottle in the step (2), performing headspace extraction at 60 ℃ for 45min, taking out the extraction head, immediately inserting into a gas chromatography sample injection port, desorbing for 5min, and performing sample injection analysis;
gas chromatography conditions: hp-5 capillary column (30 m × 0.25mm × 0.25 μm), injection inlet temperature 250 deg.C, carrier gas of high-purity helium gas greater than or equal to 99.999%, carrier gas flow rate of 1.0mL/min, temperature programming: the initial temperature is 40 ℃, the temperature is kept for 2.0min, the temperature is increased to 150 ℃ at 3 ℃/min, and then the temperature is increased to 230 ℃ at 10 ℃/min and kept for 10.0min;
mass spectrum conditions: an EI ion source; electron energy 70eV; the temperature of the four-level bar is 150 ℃, and the interface temperature is 250 ℃; electron multiplier voltage 1075V; the ion source temperature is 230 ℃; tuning in a standard manner; selecting a full scanning mode, wherein the mass scanning range is as follows: 35 to 450amu.
2. The method for constructing the fingerprint spectrum of the allspice extract for food according to claim 1, wherein the preparation of the allspice extract comprises the following steps of: cleaning allspice, drying in 40 deg.C oven for 2 hr, crushing, and sieving with 100 mesh sieve; then adding 20% ethanol water solution according to the mass ratio of 1; centrifuging the material after ultrasonic treatment, and collecting filtrate; ethanol was removed rapidly using a rotary evaporator; concentrating at low temperature to 1/5 of the original volume to obtain Pimenta dioica extract.
3. The method for constructing the fingerprint spectrum of the allspice extract for food according to claim 1, wherein 2-3g of the allspice extract in the step (2) is placed in a 20mL headspace bottle.
4. The method for constructing the fingerprint of the passion fruit extract for food according to claim 1, wherein the solid-phase microextraction extraction head is polyethylene glycol-polydimethylsiloxane, and the thickness of the coating is 100 μm.
5. The method for constructing the fingerprint of the allspice extract for food as claimed in claim 1, wherein the method for constructing the fingerprint further comprises: the gas chromatography is combined with smelling, a shunting port is arranged at the tail end of a gas chromatography column to shunt 1.
6. The method for constructing the fingerprint of the allspice extract for food according to claim 1, wherein the method for constructing the fingerprint further comprises the following steps: the Retention Index (RI) determination method comprises the steps of injecting C8-C40 normal alkane under the same analysis condition of gas chromatography-mass spectrometry, and calculating the RI value of a compound corresponding to a sample according to the retention time.
7. The method for constructing the fingerprint of the allspice extract for food as claimed in claim 1, wherein the method for constructing the fingerprint further comprises: the key flavor compound method is established, under the analysis condition of gas chromatography-mass spectrometry, the contribution of each flavor component to the overall flavor of a sample is evaluated by using a Relative Odor Activity Value (ROAV), the ROAV value of the maximum flavor contribution component of the sample is set as 100, and the ROAV calculation formula of each compound is as follows:
ROAVi≈100×Ci/Cstan×Tstan/Ti
in the formula: ROAV i Is the relative odor activity value of a certain volatile flavor substance; c i Is the relative content of certain volatile flavor substances; t is stan A threshold value that contributes the most volatile flavour substances to the odour; c stan The relative amount of the most volatile flavor that contributes to the odor; t is i Is the olfactive threshold of a certain volatile component.
When ROAV is more than or equal to l, the compound is the characteristic flavor component of the allspice extract.
8. The fingerprint of the passion fruit extract for food, which is constructed by the construction method in any one of claims 1-7.
9. The fingerprint of the allspice extract for food according to claim 8, wherein: the fingerprint spectrum of the Pimenta dioica extract has 15 common characteristic peaks, and the relative retention time of the common characteristic peaks is as follows: 12.927min, 14.594min, 15.525min, 17.993min, 21.554min, 22.213min, 25.249min, 26.550min, 30.617min, 31.153min, 32.472min, 32.703min, 33.890min, 36.606min and 41.674min, and the standard fingerprint of the allspice extract for food is obtained.
10. The fingerprint spectrum of the allspice extract for food according to claim 9, wherein the fingerprint spectrum of the allspice extract for food comprises the following characteristics: the standard fingerprint spectrum of the allspice extract has 6 characteristic flavor component peaks, and the relative retention time of the characteristic flavor component peaks is respectively as follows: 30.617min, 32.703min, 32.472min, 14.594min, 12.927min and 17.993min.
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