CN112083100A - Method for simultaneously detecting multiple volatile components in pepper or pepper product - Google Patents

Method for simultaneously detecting multiple volatile components in pepper or pepper product Download PDF

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CN112083100A
CN112083100A CN202010955854.0A CN202010955854A CN112083100A CN 112083100 A CN112083100 A CN 112083100A CN 202010955854 A CN202010955854 A CN 202010955854A CN 112083100 A CN112083100 A CN 112083100A
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pepper
volatile
temperature
volatile components
extraction
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郭添荣
张崟
吴文林
万渝平
刘文龙
张龙翼
陈代伟
朱明星
张怡
黄春燕
艾晓莉
涂松林
朱文斌
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Chengdu Food And Drug Inspection Institute
Chengdu University
Chengdu Univeristy of Technology
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Chengdu Food And Drug Inspection Institute
Chengdu University
Chengdu Univeristy of Technology
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    • G01N30/02Column chromatography
    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
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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
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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
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    • G01N30/06Preparation
    • G01N2030/062Preparation extracting sample from raw material

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Abstract

The invention provides a method for simultaneously detecting multiple volatile components in pepper or pepper products. The method adopts headspace solid phase microextraction and combines a gas chromatography-mass spectrometry technology to detect volatile components in the capsicum or capsicum products, and comprises the following steps: extracting volatile components of the pepper or the pepper product by using a solid phase micro-extraction instrument; injecting the obtained volatile components into a gas chromatography-mass spectrometer for detection to obtain a total ion current chromatogram map; and comparing and analyzing the obtained total ion current chromatogram with a standard chromatogram to obtain the composition and content of volatile components in the pepper or pepper product. The detection method can simultaneously carry out qualitative and quantitative analysis on various volatile components in the pepper or pepper products, is very important for controlling the processing technology of the pepper products (particularly the crispy pepper) and preparing the pepper products which have no toxic volatile aroma components and rich content and do not contain toxic volatile substances, and has wide application prospect.

Description

Method for simultaneously detecting multiple volatile components in pepper or pepper product
Technical Field
The invention belongs to the technical field of analysis and detection, and particularly relates to a method for simultaneously detecting multiple volatile components in hot peppers or hot pepper products (particularly crispy chili).
Background
The capsicum is a herbaceous vegetable belonging to the solanaceae family, and not only is rich in various vitamins, but also contains a large amount of carotene, folic acid, mineral substances and other substances, and the substances are essential nutrient components for human bodies. It has been popular with consumers for a long time because of its functions of promoting appetite and digestion, warming stomach and dispelling cold, promoting blood circulation, etc.
The pepper has larger taste and is not suitable for direct eating, and the crisp fried pepper is a main way for improving the taste of the pepper. The fried crispy pepper is prepared by using fresh pepper as a raw material, cleaning the fresh pepper, removing bases, draining surface water, and drying. The fried crispy pepper can be directly eaten by consumers, and can also be used as an important material for processing flavor food, so that the flavor of the food is improved in a seasoning mode. Therefore, the flavor of the fried crispy pepper directly affects the quality of the flavored food.
During the shortening process, the peppers can generate a plurality of volatile aroma components to increase the aroma and the taste of the shortening peppers, but are easy to generate highly toxic substances (such as 2, 4-decadienal) which are harmful to human health.
Therefore, a method capable of effectively detecting the types and the contents of volatile aroma components and toxic substances in the crispy chili is researched, and the method is very important for controlling the crispy chili process and preparing the crispy chili with the types of nontoxic volatile aroma components, rich contents, and less toxic volatile substances.
Headspace solid phase microextraction in combination with gas chromatography-mass spectrometry (HS-SPME-GC-MS) is a method that combines headspace solid phase microextraction, gas chromatography, and mass spectrometry to detect volatile components. The method comprises the steps of firstly extracting volatile components of a substance to be detected by using a headspace solid phase microextraction technology (HS-SPME), and then detecting by using gas chromatography-mass spectrometry (GC-MS). Compared with other common extraction methods (such as microwave-assisted extraction steam extraction method, normal-pressure and reduced-pressure steam distillation method, organic solvent extraction method and simultaneous distillation extraction method), the headspace solid phase microextraction is simple, rapid, economic and safe, good in selectivity and high in sensitivity, integrates sampling, extraction, concentration and sample injection, greatly accelerates analysis and detection speed, is not easily influenced by external environment in the extraction process, and has complete and reliable detected aroma components and content.
However, at present, no report is found for simultaneously detecting various volatile aroma components and volatile toxic substances in the crispy chili by utilizing headspace solid-phase microextraction in combination with a gas chromatography-mass spectrometry.
Disclosure of Invention
The invention aims to provide a method for simultaneously detecting multiple volatile aroma components and volatile toxic substances in pepper or pepper products (particularly crispy chili) based on headspace solid-phase microextraction combined with a gas chromatography-mass spectrometry technology.
The invention provides a method for simultaneously detecting multiple volatile components in pepper or pepper products, which comprises the following steps: adopting headspace solid phase microextraction and combining with gas chromatography-mass spectrometry technology to detect volatile components in the pepper or pepper products, comprising the following steps:
(1) extracting volatile components of the pepper or the pepper product by using a solid phase micro-extraction instrument;
(2) injecting the volatile components obtained in the step (1) into a gas chromatography-mass spectrometer for detection to obtain a total ion current chromatogram;
(3) and (3) comparing and analyzing the total ion current chromatogram obtained in the step (2) with a standard spectrogram to obtain the composition of volatile components in the hot pepper or the hot pepper product.
Further, the method further comprises the steps of:
(4) and (3) quantitatively analyzing the total ion current chromatogram obtained in the step (2) by using a peak area normalization method to obtain the content of each volatile component in the hot pepper or the hot pepper product.
Further, in the step (2), the gas chromatography conditions are as follows:
a chromatographic column: methyl polysiloxane is taken as a filler, preferably, the methyl polysiloxane is (5% -phenyl) -methyl polysiloxane, and more preferably HP-5 MS;
mobile phase: an inert gas; preferably, the inert gas is helium, and the flow rate is 1 mL/min;
the temperature of a sample inlet is 200-300 ℃, and preferably 250 ℃;
the temperature-raising program is set as follows: maintaining the initial temperature at 40 deg.C for 5 min; heating to 160 deg.C at 4 deg.C/min, and maintaining for 5 min; then the temperature is raised to 250 ℃ at the speed of 6 ℃/min and kept for 5 min.
Further, in step (2), the mass spectrometry conditions are: the ion source type EI is characterized in that the electron energy is 70eV, the ion source temperature is 200-250 ℃, and the preferred temperature is 230 ℃; the interface temperature is 200-250 ℃, and preferably 230 ℃; the temperature of the four-level bar is 130-170 ℃, and preferably 150 ℃; the mass scanning range is 35-450 amu.
Further, in the step (1), the volatile components comprise volatile aroma components and volatile toxic components; preferably, the volatile aroma components comprise one or more of furan formaldehyde, p-xylene, 5-methylfuran aldehyde, 2-pyrrole formaldehyde, 2-acetyl pyrrole, linalool, 1-methylpyrrole-2-carboxylic acid, p-methylacetophenone, trans-2-decenal, o-isopropylthiophenol, anethole, tetrahydro-2-octylfuran, trans-2, 4-decadienal, 1, 6-trimethyl-1, 2-dihydronaphthalene, trans-2-dodecenal, pyrinol ester, allomyrcene and dihydroactinidiolide, and the volatile toxic components comprise 2, 4-decadienal.
Further, in the step (1), the pepper product is fried crispy pepper; preferably, the crispy chili is prepared by the following method: adding the hot pepper into oil, and frying for 30-60 seconds at 130-170 ℃.
Further, the temperature of the shortening is 170 ℃, the time of the shortening is 40-50 seconds, preferably, the temperature of the shortening is 170 ℃, and the time of the shortening is 40 seconds;
and/or the mass volume ratio of the pepper to the oil is 1 (2-5) g/mL, preferably 1:3 g/mL;
and/or, the pepper is dried pepper, preferably seven-star dried pepper;
and/or the oil is a vegetable or animal oil, preferably a vegetable oil.
Further, in the step (1), the extraction method comprises the following steps: adding water or aqueous solution into Capsici fructus or Capsici fructus product, placing in a headspace bottle of solid phase micro-extraction apparatus, heating and stirring, inserting the extraction head of the solid phase micro-extraction apparatus into the headspace bottle, and performing headspace extraction.
Further, in the step (1), the mass-to-volume ratio of the pepper or the pepper product to water or the water solution is 0.1-10 g/mL, preferably 1 g/mL; and/or the aqueous solution is an aqueous NaCl solution, preferably a saturated aqueous NaCl solution; and/or, prior to placing in the headspace bottle, further comprising vortexing; and/or the heating and stirring temperature is 50-70 ℃, preferably 65 ℃, and the time is 5-30 min, preferably 15 min; and/or the extraction head is positioned 0.5-2.0 cm above the liquid level of the headspace bottle, preferably 1.0cm above the liquid level; and/or the extraction conditions are as follows: heating to 75-85 ℃ under a stirring state, and extracting for 20-40 min, preferably, the heating temperature is 80 ℃, and the extraction time is 30 min.
Further, in the step (2), the detection method is as follows: taking out the extraction head after the headspace extraction in the step (1), inserting the extraction head into a sample inlet of a gas chromatography-mass spectrometer, desorbing, starting the gas chromatography-mass spectrometer, and starting detection; preferably, the desorption temperature is 200-300 ℃, preferably 250 ℃, and the time is 3-10 min, preferably 5 min.
The headspace bottle is a device adapted to be used in a solid phase microextraction apparatus.
In the invention, the shortening refers to a processing process of putting food into oil and heating the food at a certain temperature to react.
Experimental results show that by utilizing the headspace solid-phase microextraction combined with the gas chromatography-mass spectrometry technology, the composition and content of various volatile aroma components and toxic components (such as 2, 4-decadienal) in the raw material dried pepper and the crispy dried pepper prepared by different processes can be successfully detected under the specific chromatographic conditions and mass spectrometry conditions. By utilizing the detection method, the optimal conditions for preparing the crispy dried chili are screened out: the temperature of the shortening is 170 ℃, and the shortening time is 40 s.
Compared with the raw material dried pepper, the types of the aroma components of the obtained fried dried pepper are obviously increased under the optimal conditions (the temperature of the fried cake is 170 ℃ and the time of the fried cake is 40s), and the types of the aroma components are more abundant.
Compared with the crispy dried peppers obtained under other crispy conditions, the crispy dried peppers obtained under the preferable conditions (the temperature of the crispy cake is 170 ℃, the time of the crispy cake is 40s) have obviously increased types and contents of aroma components and do not contain 2, 4-decadienal which is a highly toxic component.
The detection method can effectively detect the composition and content of various volatile aroma components and toxic substances in the pepper and pepper products, can perform qualitative and quantitative analysis on various volatile components in the pepper or pepper products simultaneously, and is very important for controlling the processing technology of the pepper products (particularly crispy fried pepper) to prepare the pepper products which are rich in the types and content of nontoxic volatile aroma components and do not contain toxic volatile substances, and the application prospect is wide.
Obviously, many modifications, substitutions, and variations are possible in light of the above teachings of the invention, without departing from the basic technical spirit of the invention, as defined by the following claims.
The present invention will be described in further detail with reference to the following examples. This should not be understood as limiting the scope of the above-described subject matter of the present invention to the following examples. All the technologies realized based on the above contents of the present invention belong to the scope of the present invention.
Drawings
FIG. 1 is a total ion flow chromatogram of the volatile components of sample A.
FIG. 2 is a total ion flow chromatogram of the volatile components of sample B.
FIG. 3 is a total ion current chromatogram of the volatile components of sample C.
Detailed Description
The raw materials and equipment used in the invention are known products and are obtained by purchasing commercial products.
The dry pepper adopted in the embodiment of the invention is the market-sold seven-star pepper dry pepper, and has red and bright color, no worm damage, no mildew and no damage.
An experimental instrument: solid phase microextraction instrument (HP-1510, containing 65 μm PDMS/DVB extraction head, Supelco, USA); gas chromatography-mass spectrometer (GC-MS, Agilent 7890B/5977A, Agilent Inc. USA); chromatography column (HP-5MS, 30 m.times.250. mu.m.times.0.25. mu.m, Agilent, USA).
Example 1: method for detecting volatile aroma components and toxic substances in crispy chili based on headspace solid-phase microextraction combined with gas chromatography-mass spectrometry technology
1. Preparation of samples to be tested
(A) Taking 1.5kg of dried pepper, washing with clear water, drying in the air, cutting fruit stalks, and cutting into small sections with the length of about 1cm for later use.
(B) 1.5kg of dried pepper is taken, washed by clear water and dried, and the stem is cut off and cut into small sections with the length of about 1 cm. Taking 500g of dried peppers cut into small sections, placing the dried peppers into an automatic temperature control butter crunchy pan filled with vegetable oil, wherein the mass volume ratio of the dried peppers to the vegetable oil is 1:3g/mL, frying the mixture for 40s at 170 ℃, and taking out the mixture to obtain the fried and crisp dried chili for later use.
(C) 1.5kg of dried pepper is taken, washed by clear water and dried, and the stem is cut off and cut into small sections with the length of about 1 cm. Taking 500g of dried peppers cut into small sections, placing the dried peppers into an automatic temperature control butter crunchy pan filled with vegetable oil, wherein the mass volume ratio of the dried peppers to the vegetable oil is 1:3g/mL, frying the fried dough cake for 90s at 210 ℃, and taking out to obtain the fried dough cake dry chili for later use.
2. Headspace solid phase microextraction and gas chromatography-mass spectrometry combined detection
Accurately weighing A, B, C g (accurate to 0.1g) of the sample to be tested, respectively adding 5mL of saturated NaCl solution, vortex shaking for 3min, placing in a 15mL headspace bottle, and heating and balancing on a magnetic stirrer at 65 ℃ for 15 min. Inserting a 65-micron PDMS/DVB activated extraction head (250 ℃, 45min) into a headspace bottle, positioning the extraction head at a position 1cm above the liquid level in the headspace bottle, stirring at 1000r/min, heating to 80 ℃, taking out the extraction head after headspace extraction for 30min, quickly inserting the extraction head into a gas chromatograph sample inlet of a GC-MS instrument, desorbing for 5min at 250 ℃, starting the GC-MS instrument and collecting data to obtain a total ion current chromatogram.
Chromatographic conditions are as follows: a chromatographic column: agilent HP-5MS (30m is multiplied by 250 μm is multiplied by 0.25 μm), helium is taken as carrier gas in the instrument, the linear flow rate is 1mL/min, the injection inlet temperature is 250 ℃, the desorption time is 5min, and the sample injection is carried out in a non-shunting mode. The sample is injected without shunting, and the sample injection amount is 1 mu L. Setting the temperature raising program to be the initial temperature of 40 ℃, and keeping for 5 min; heating to 160 deg.C at 4 deg.C/min, and maintaining for 5 min; then the temperature is raised to 250 ℃ at the speed of 6 ℃/min and kept for 5 min.
Mass spectrum conditions: ion source type EI, electron energy 70 eV; the ion source temperature and the interface temperature are both 230 ℃; the quadrupole temperature was 150 ℃. And a full SCAN mode (SCAN) is adopted, and the mass SCAN range is 35-450 amu.
3. Data processing and analysis
By utilizing MassHunter GC/MS Acquisition Software (B.07.00) and MSD ChemStation Data Analysis (F.01.00) Data Analysis Software matched with an Agilent 7890B/5977A gas chromatography-mass spectrometer system, after Data Acquisition is finished, analyzing a primary mass spectrum and a secondary mass spectrum of each component according to automatically retrieving and matching each peak structural formula in a Data Analysis spectrum, contrasting the primary mass spectrum and the secondary mass spectrum with a standard spectrum, and qualitatively analyzing each component by combining a retention index; and (4) carrying out quantitative analysis on the content of each component by adopting a peak area normalization method.
4. Analysis results
4.1 comparison of volatile aroma and toxic ingredients of dried Capsici fructus and Fried and crisp dried Capsici fructus
The total ion current chromatogram of sample A, B, C is shown in FIGS. 1-3. The analysis and comparison of each peak in the total ion current chromatogram confirm that the results are shown in table 1.
TABLE 1 comparison of volatile aroma and toxic components for sample A, B, C
Figure BDA0002678560600000051
As is clear from Table 1, volatile components in the shortening dried peppers (sample B, C) obtained under different shortening conditions were mainly aldehydes, alkenes, esters, alcohols, alkanes, phenols, and the like. In terms of species, 20 kinds of volatile compounds were detected in the raw dried capsicum before shortening (sample a), and 18 kinds and 26 kinds of volatile compounds were detected in the group B dried capsicum and the group C dried capsicum. The volatile components in sample A, B, C varied widely, with different types, amounts and relative amounts of compounds.
By utilizing the headspace solid-phase microextraction combined with the gas chromatography-mass spectrometry analysis method, volatile aroma components and toxic substances of the obtained crispy dried chili under different crispy conditions can be detected. By utilizing the headspace solid-phase microextraction and combining with a gas chromatography-mass spectrometry analysis method, the shortening process of the capsicum can be regulated and controlled, and the crispy capsicum which is nontoxic, rich in volatile aroma component types and contents and does not contain toxic volatile substances is prepared.
The following are specific analysis results of volatile components in each sample.
4.2 volatile component analysis of sample A
TABLE 2 volatile constituents in sample A
Figure BDA0002678560600000061
As can be seen from table 2, the volatile substances detected in the raw material dried pepper before shortening (sample a) were 20 kinds, and mainly included 3 kinds of aldehydes, 4 kinds of alkenes, 4 kinds of alcohols, 2 kinds of benzene rings, 3 kinds of esters, 1 kind of phenols, 2 kinds of ketones, and 1 kind of alkanes. The raw material of the dried pepper contains no 2, 4-decadienal which is a highly toxic component.
The raw material of the dried pepper has only four volatile components which present aroma and have high content: linalool (40.69%), anethole (19.39%), valerian-4, 7(11) -diene (15.76%), linalyl acetate (8.70%).
4.3 volatile component analysis of sample B
TABLE 3 sample group B volatile Components
Figure BDA0002678560600000071
As can be seen from table 3, the volatile substances detected in sample B are 18 in total, and mainly include 6 aldehydes, 2 alkenes, 1 alcohol, 1 benzene ring, 3 esters, 1 phenol, 1 ketone, 1 alkane, and 2 heterocycles. Sample B contained no highly toxic 2, 4-decadienal.
The sample B presents fragrance, the content of volatile components is higher than 8, and the types of the fragrance components are richer than those of the raw material dry pepper; the 8 aroma components are as follows: trans 2, 4-decadienal (18.97%), 5-methylfuran aldehyde (10.82%), linalool (10.38%), allo-myrcene (7.25%), trans-2-dodecenal (7.17%), anisene (6.83%), furfural (6.30%), p-xylene (5.51%).
4.4 volatile component analysis of sample C
TABLE 4 volatile constituents in sample C
Figure BDA0002678560600000072
Figure BDA0002678560600000081
As can be seen from table 4, the volatile substances detected in sample C total 26, and mainly include 8 aldehydes, 5 alkenes, 3 alcohols, 2 esters, 4 ketones, 1 alkane, and 3 heterocycles. Sample C yielded a highly toxic component, 2, 4-decadienal (7.83%).
In the sample C, only 6 volatile components which present fragrance and have high content are available, and the types of the fragrance components are not as rich as those of the sample B; the 6 aroma components are respectively: 2-acetylpyrrole (12.21%), linalool (11.72%), 2, 3-dihydro-3, 5-dihydroxy-6-methyl-4 (H) -pyran-4-one (11.13%), linalyl acetate (10.37%), anethole (9.78%) beta-ionone (6.68%).
The experimental results show that after the dried chili raw material is treated by different shortening processes, the obtained fried crispy dried chili has great difference of volatile aroma components and toxic components. Compared with the raw material dried pepper, the types of volatile aroma components of the obtained fried dried pepper are obviously increased under the specific conditions of the crisps (the temperature of the crisps is 170 ℃ and the time of the crisps is 40s), and the types of the volatile aroma components are richer. Compared with the crispy dried chili obtained under other crispy conditions (the temperature of the crispy is 210 ℃ and the time of the crispy is 90s), the crispy dried chili obtained under the specific crispy conditions (the temperature of the crispy is 170 ℃ and the time of the crispy is 40s) has obviously increased types and contents of volatile aroma components and does not contain 2, 4-decadienal which is a highly toxic component.
Therefore, by using the headspace solid-phase microextraction combined with the gas chromatography-mass spectrometry technology of the embodiment, under the specific chromatographic conditions and mass spectrometry conditions of the invention, the composition and content of various volatile aroma components and toxic components (such as 2, 4-decadienal) in the raw dried peppers and the crispy dried peppers prepared by different processes can be successfully detected at the same time. Under the detection method of the embodiment, a preferable condition for preparing the crispy dried chili is selected: the temperature of the shortening is 170 ℃, and the shortening time is 40 s.
In conclusion, the invention provides a method for simultaneously detecting various volatile components in the crispy chili based on headspace solid-phase microextraction combined with gas chromatography-mass spectrometry, and under the specific chromatographic conditions and mass spectrometry conditions of the invention, the composition and content of various volatile aroma components and toxic components (such as 2, 4-decadienal) in the raw material dried chili and the crispy dried chili prepared by different processes can be simultaneously and successfully detected. The detection method is very important for controlling the processing technology of the pepper products (particularly the crispy pepper) and preparing the pepper products which have the advantages of rich types and contents of nontoxic volatile aroma components, no toxic volatile substances and wide application prospect.

Claims (10)

1. A method for simultaneously detecting multiple volatile components in a pepper or pepper product, comprising: the method comprises the following steps: adopting headspace solid phase microextraction and combining with gas chromatography-mass spectrometry technology to detect volatile components in the pepper or pepper products, comprising the following steps:
(1) extracting volatile components of the pepper or the pepper product by using a solid phase micro-extraction instrument;
(2) injecting the volatile components obtained in the step (1) into a gas chromatography-mass spectrometer for detection to obtain a total ion current chromatogram;
(3) and (3) comparing and analyzing the total ion current chromatogram obtained in the step (2) with a standard spectrogram to obtain the composition of volatile components in the hot pepper or the hot pepper product.
2. The method of claim 1, wherein: the method further comprises the steps of:
(4) quantitatively analyzing the total ion current chromatogram obtained in the step (2) of claim 1 by using a peak area normalization method to obtain the content of each volatile component in the pepper or the pepper product.
3. The method according to any one of claims 1 to 2, wherein: in the step (2), the gas chromatography conditions are as follows:
a chromatographic column: methyl polysiloxane is taken as a filler, preferably, the methyl polysiloxane is (5% -phenyl) -methyl polysiloxane, and more preferably HP-5 MS;
mobile phase: an inert gas; preferably, the inert gas is helium, and the flow rate is 1 mL/min;
the temperature of a sample inlet is 200-300 ℃, and preferably 250 ℃;
the temperature-raising program is set as follows: maintaining the initial temperature at 40 deg.C for 5 min; heating to 160 deg.C at 4 deg.C/min, and maintaining for 5 min; then the temperature is raised to 250 ℃ at the speed of 6 ℃/min and kept for 5 min.
4. The method according to any one of claims 1 to 2, wherein: in the step (2), the mass spectrum conditions are as follows: the ion source type EI is characterized in that the electron energy is 70eV, the ion source temperature is 200-250 ℃, and the preferred temperature is 230 ℃; the interface temperature is 200-250 ℃, and preferably 230 ℃; the temperature of the four-level bar is 130-170 ℃, and preferably 150 ℃; the mass scanning range is 35-450 amu.
5. The method according to any one of claims 1 to 4, wherein: in the step (1), the volatile components comprise volatile aroma components and volatile toxic components; preferably, the volatile aroma components comprise one or more of furan formaldehyde, p-xylene, 5-methylfuran aldehyde, 2-pyrrole formaldehyde, 2-acetyl pyrrole, linalool, 1-methylpyrrole-2-carboxylic acid, p-methylacetophenone, trans-2-decenal, o-isopropylthiophenol, anethole, tetrahydro-2-octylfuran, trans-2, 4-decadienal, 1, 6-trimethyl-1, 2-dihydronaphthalene, trans-2-dodecenal, pyrinol ester, allomyrcene and dihydroactinidiolide, and the volatile toxic components comprise 2, 4-decadienal.
6. The method according to any one of claims 1 to 4, wherein: in the step (1), the pepper product is fried crispy pepper; preferably, the crispy chili is prepared by the following method: adding the hot pepper into oil, and frying for 30-60 seconds at 130-170 ℃.
7. The method of claim 6, wherein: the temperature of the shortening is 170 ℃, the time of the shortening is 40-50 seconds, preferably, the temperature of the shortening is 170 ℃, and the time of the shortening is 40 seconds;
and/or the mass volume ratio of the pepper to the oil is 1 (2-5) g/mL, preferably 1:3 g/mL;
and/or, the pepper is dried pepper, preferably seven-star dried pepper;
and/or the oil is a vegetable or animal oil, preferably a vegetable oil.
8. The method according to any one of claims 1 to 4, wherein: in the step (1), the extraction method comprises the following steps: adding water or aqueous solution into Capsici fructus or Capsici fructus product, placing in a headspace bottle of solid phase micro-extraction apparatus, heating and stirring, inserting the extraction head of the solid phase micro-extraction apparatus into the headspace bottle, and performing headspace extraction.
9. The method according to claims 1 to 4, wherein: in the step (1), the mass-to-volume ratio of the pepper or the pepper product to water or an aqueous solution is 0.1-10 g/mL, preferably 1 g/mL; and/or the aqueous solution is an aqueous NaCl solution, preferably a saturated aqueous NaCl solution; and/or, prior to placing in the headspace bottle, further comprising vortexing; and/or the heating and stirring temperature is 50-70 ℃, preferably 65 ℃, and the time is 5-30 min, preferably 15 min; and/or the extraction head is positioned 0.5-2.0 cm above the liquid level of the headspace bottle, preferably 1.0cm above the liquid level; and/or the extraction conditions are as follows: heating to 75-85 ℃ under a stirring state, and extracting for 20-40 min, preferably, the heating temperature is 80 ℃, and the extraction time is 30 min.
10. The method of claim 9, wherein: in the step (2), the detection method comprises the following steps: taking out the extraction head after the headspace extraction in the step (1), inserting the extraction head into a sample inlet of a gas chromatography-mass spectrometer, desorbing, starting the gas chromatography-mass spectrometer, and starting detection; preferably, the desorption temperature is 200-300 ℃, preferably 250 ℃, and the time is 3-10 min, preferably 5 min.
CN202010955854.0A 2020-09-11 2020-09-11 Method for simultaneously detecting multiple volatile components in pepper or pepper product Pending CN112083100A (en)

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