CN115343429A - Method for detecting volatile flavor substances in spice oil based on PCA (principal component analysis) analysis technology and application - Google Patents
Method for detecting volatile flavor substances in spice oil based on PCA (principal component analysis) analysis technology and application Download PDFInfo
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- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N33/00—Investigating or analysing materials by specific methods not covered by groups G01N1/00 - G01N31/00
- G01N33/02—Food
- G01N33/03—Edible oils or edible fats
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
- G01N21/17—Systems in which incident light is modified in accordance with the properties of the material investigated
- G01N21/25—Colour; Spectral properties, i.e. comparison of effect of material on the light at two or more different wavelengths or wavelength bands
- G01N21/31—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry
- G01N21/33—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry using ultraviolet light
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Abstract
The invention relates to a method for detecting volatile flavor substances in spice oil based on PCA (principal component analysis) analysis technology, which comprises the following steps: (1) preparing a spice oil sample; (2) Selecting Heracles II ultra-fast gas-phase electronic nose to measure the volatile flavor substances of the spice oil sample; (3) Carrying out statistical analysis on the measurement data of the volatile flavor substances by utilizing a PCA method; (4) The method is applied to preparation and processing procedures of the zanthoxylum flavor oil, indexes such as color, acid value, peroxide value, zanthoxylum amide, fatty acid and the like of the zanthoxylum flavor oil are analyzed around each processing procedure, volatile flavor substances in each procedure in the processing process of the zanthoxylum flavor oil are monitored by using a HeracleisI ultra-fast gas-phase electronic nose, key technical control points in the processing process of the zanthoxylum flavor oil are determined by closely combining production lines of enterprises, so that theoretical guidance is provided for grease quality control of zanthoxylum flavor oil production enterprises in future, and the method has important conversion application value.
Description
Technical Field
The invention belongs to the field of food processing, relates to an oil detection technology, and particularly relates to a spice oil volatile flavor substance detection method based on a PCA analysis technology and application thereof.
Background
The spice is a spice component contained in natural plants, has special smell and taste, can endow a product with certain flavor, can inhibit or correct the bad smell of food, is an ideal food processing ingredient, and the flavor of spice seasoning oil is important for quality evaluation and the degree of preference of consumers. At present, the detection methods of volatile flavor substances of spice seasoning oil mainly comprise an electronic nose, a gas chromatography-mass spectrometry and the like.
The prior publications describe a method for simultaneously detecting a plurality of volatile components in pepper or pepper products (CN 112083100 a) and a method for analyzing and identifying a pepper oil flavor characteristic index compound (CN 106053653A), but these methods detect and identify volatile flavor substances of pepper seasoning oil prepared by using vegetable oil as base oil, and have few disclosures on methods for detecting and identifying animal fat volatile flavor substances, and no disclosure on a method for detecting volatile flavor substances of spice oil based on PCA analysis technology.
Disclosure of Invention
The invention aims to overcome the defects of the prior art, provides a spice oil volatile flavor substance detection method based on a PCA analysis technology, applies the method to the preparation process of pepper flavor oil, researches and compares the influence of different processing procedures on the quality change of pepper seasoning oil and the PCA analysis result, has important significance for the flavor detection of animal fat spice oil, and can also develop new research and design ideas for the quality control of spice seasoning oil and the product upgrading.
The technical problem to be solved by the invention is realized by adopting the following technical scheme:
a method for detecting volatile flavor substances in spice oil based on PCA analysis technology comprises the following steps:
(1) Spice oil sample preparation
Heating raw oil to 180 ℃, pouring the raw oil into an extraction tank filled with carefully selected and crushed spices, stirring the raw oil once every 5min by using a stirring rod for 30min, soaking the raw oil in the extraction tank for 3-4 days to ensure that the spices are fully extracted, filtering an upper oil sample by using a plate type closed filter after soaking, and clarifying the filtered oil sample in a storage tank to obtain a final finished oil sample;
(2) Performing index measurement and volatile flavor substance measurement on the spice oil sample, wherein Heracles II ultra-fast gas phase electronic nose is selected for detection in the volatile flavor substance measurement;
the index determination of the spice oil sample comprises the following steps: amide compound determination, color determination, acid value determination, peroxide value determination and fatty acid determination.
The method for determining the amide compounds comprises the following steps:
(1) Standard curve creation
Taking 5mg of a hydroxy-beta-sanshool standard substance, diluting to 5mL with methanol to obtain a hydroxy-beta-sanshool standard solution, respectively sucking 0, 1, 2, 3, 4, 5, 6, 7 and 8mL of standard solutions, preparing a hydroxy-beta-sanshool solution with the concentration of 0-8 mu g/mL with methanol, measuring the absorbance at 267nm, and drawing a standard curve by taking the concentration as a horizontal coordinate and the absorbance value as a vertical coordinate;
(2) Zanthoxylum bungeanum amide determination
Measuring the content of the Zanthoxylum bungeanum amide by referring to a method in appendix A of DBS51/008-2019 food safety local standard Zanthoxylum oil, calculating the content of the hydroxyl-beta-sanshool according to a standard curve, wherein a regression equation is y =0.1501x-0.1288 2 =0.9983 where y is the absorbance value and x is the zanthoxylum amide content.
The volatile flavor substance is detected by using Heracles II ultra-fast gas phase electronic nose, the detection method comprises the steps of taking 2g of spice oil samples in a 20mL headspace bottle, preheating for 24min in a 55 ℃ water bath kettle, manually injecting samples, and paralleling 3 samples.
(3) Carrying out statistical analysis on the measurement data of the volatile flavor substances by using a PCA (principal component analysis) method, wherein the detection parameters are as follows: the sample inlet temperature is 200 ℃, the sample volume is 5000 mu L, the injection speed is 125 mu L/s, the sample introduction time is 45s, the trap initial temperature is 40 ℃, the shunt rate is 10mL/min, the final temperature is 200 ℃, the initial column temperature is 50 ℃, the temperature is increased to 80 ℃ at 1 ℃/s, then the temperature is increased to 250 ℃ at 3 ℃/s, the collection time is 110s, and the FID detector temperature is 260 ℃.
(4) And (4) analyzing the distinguishing index, wherein the distinguishing index is calculated based on the relative distance between the gravity centers of the two sample groups in the PCA diagram, the larger the distance between the two sample groups is, the smaller the difference in the groups is, and the closer the distinguishing index is to 100 percent, namely, the distinguishing index is positively correlated with the difference between the samples.
The spice oil volatile flavor substance detection method based on the PCA analysis technology is applied to vegetable zanthoxylum oil, and PCA analysis is respectively carried out on crude oil before extraction, an oil sample for 24 hours after extraction, an oil sample for 72 hours after extraction, a plate-frame filtration oil sample, a clarified oil sample and finished oil.
The PCA method is applied to the processing process of the pepper seasoning oil in the vegetable pepper oil, the odor difference among samples in each process is obvious, 8 volatile flavor substances including hexanal, nonanal, heptanal, (E, E) -2,4-heptadienal are detected in the soybean oil, and 13 volatile flavor substances including alcohols and olefins are detected in the pepper seasoning oil.
The PCA method analysis shows that the variance contribution rate of the first principal component is 90.083%, the variance contribution rate of the second principal component is 8.299%, the cumulative total contribution rate of the first principal component and the second principal component is 98.382%, the identification index among samples is 95, and the distance among the samples in a PCA analysis chart is in positive correlation with the odor difference among the samples.
The invention has the advantages and positive effects that:
the invention has scientific and reasonable design, provides a spice oil volatile flavor substance detection method based on PCA analysis technology, applies the method to the preparation and processing procedures of the prickly ash flavor oil, uses Heracles II ultra-fast gas-phase electronic nose to monitor volatile flavor substances among the procedures in the processing process of the prickly ash flavor oil around the influence of the processing procedures on indexes such as color, acid value, peroxide value, zanthoxylamide, fatty acid and the like of the prickly ash flavor oil, researches the quality and aroma change in the processing process of the prickly ash flavor oil, closely combines the production line of an enterprise, determines key control points in the processing process of the prickly ash flavor oil, and provides theoretical guidance for grease quality control of a prickly ash flavor oil production enterprise in the future, and has important conversion and application values.
Drawings
FIG. 1 is a flow chart of the production process of zanthoxylum oil in the invention;
FIG. 2 shows the result of the change of acid value during the processing of the zanthoxylum bungeanum seasoning oil in the embodiment of the invention;
FIG. 3 shows the result of the change of peroxide value during the processing of the zanthoxylum bungeanum seasoning oil in the embodiment of the invention;
FIG. 4 shows the results of the changes in the content of Zanthoxylum piperitum amide during the processing of the Zanthoxylum bungeanum flavoring oil in the example of the present invention;
FIG. 5 is a graph of the PCA analysis among samples during the processing of zanthoxylum bungeanum seasoning oil in the example of the present invention.
Detailed Description
The present invention is further described in the following examples, which are intended to be illustrative, not limiting and are not intended to limit the scope of the invention.
The invention provides a spice oil volatile flavor substance detection method based on a PCA analysis technology and application thereof, and particularly provides a spice oil volatile flavor substance detection method based on a PCA analysis technology, and the method is applied to the preparation process of pepper flavor oil, and the influence of different processing procedures on the quality change of pepper flavor oil and PCA analysis are researched and compared.
The experimental pepper is green pepper and purchased from Sichuan Manyu green commercial company Limited; soybean oil was purchased from Shandong Yu Wang Shengtai food industries, inc. The zanthoxylum oil used in the experiment is sampled from Hongluo food Limited company in Tianjin, and the sampling points are crude oil before extraction, extraction for 24 hours, extraction for 72 hours, plate-frame filtration, clarification and finished product.
Glacial acetic acid and 95% ethanol are analytically pure and purchased from Tianjin, tianli chemical reagent company; phenolphthalein indicator, methanolic potassium iodide: the analytical reagent is purchased from the Dalochi chemical reagent factory in Tianjin; the chloroform is analytically pure and purchased from chemical reagent supply and sale company in Tianjin; soluble starch, 0.1mol/L sodium hydroxide standard titration solution and 0.01009mol/L sodium thiosulfate standard titration solution are purchased from Tianjin chemical reagent three factories; hydroxy-beta-sanshool was purchased from Shanghai leaf Biotech limited.
Apparatus and devices relate to: model HZ-K500C electronic balance: shanghai youke instruments and meters ltd; heracleisI ultra-fast gas phase electronic nose: french Alpha m.o.s company; UV-800 UV-vis spectrophotometer: hmadzu corporation, japan; CM-5 type color difference meter: shenzhen, san Enz science and technology Limited; agilent 7890A gas chromatograph: agilent, USA.
The specific experimental method comprises the following steps:
1. preparation of pepper flavor oil
The production enterprise of oleum Zanthoxyli Bungeani heats soybean oil to 180 deg.C, pours into the extraction tank containing selected and pulverized fructus Zanthoxyli, and stirs the raw materials in the extraction tank with a special stirring rod once every 5min for 30min. Soaking the oil in the leaching tank for 3-4 days to fully leach out the aroma. And filtering the upper oil sample by using a high-efficiency plate-type closed filter after soaking, and clarifying the filtered oil sample in a storage tank to obtain a final finished product. The process flow is shown in figure 1.
2. Determination of amide Compounds
(1) Standard curve establishment
Taking 5mg of a hydroxy-beta-sanshool standard substance, diluting to 5mL with methanol to obtain a hydroxy-beta-sanshool standard solution, sucking 0, 1, 2, 3, 4, 5, 6, 7 and 8mL of standard solution respectively, preparing a 0-8 mu g/mL hydroxy-beta-sanshool solution with methanol, and measuring the absorbance at 267 nm. And drawing a standard curve by taking the concentration as an abscissa and the absorbance value as an ordinate.
(2) Zanthoxylum bungeanum amide determination
Measuring the content of the Zanthoxylum bungeanum amide by referring to a method in appendix A of DBS51/008-2019 food safety local standard Zanthoxylum oil, calculating the content of the hydroxy-beta-sanshool according to a standard curve, and obtaining a regression equation of y =0.1501x-0.1288 (R) 2 = 0.9983) where y is the absorbance value and x is the zanthoxylum amide content.
(3) Determination of volatile flavor substances
And (3) detecting volatile flavor substances of samples among processing procedures of the pepper seasoning oil by using a Heracles II ultra-fast gas-phase electronic nose.
Weighing 2g of pepper seasoning oil at several sampling points before leaching (crude oil), leaching (24 h), leaching (72 h), plate-frame filtering, clarifying, and finishing, placing in a 20mL headspace bottle, preheating in a 55 ℃ water bath for 24min, manually injecting samples, and making 3 samples in parallel.
Detecting parameters: the injection port temperature is 200 ℃, the injection volume is 5000 mu L, the injection speed is 125 mu L/s, and the injection time is 45s. The trap initial temperature was 40 ℃, the shunt rate was 10mL/min, and the final temperature was 200 ℃. Initial column temperature 50 ℃, 1 ℃/s to 80 ℃, 3 ℃/s to 250 ℃, acquisition time 110s, fid detector temperature 260 ℃.
Experimental results and data analysis
1. Influence of processing procedures on color and luster of pepper seasoning oil
The color change of the pepper seasoning oil in the processing process is shown in table 1, and as can be seen from table 1, the L value of the pepper seasoning oil is lower when the pepper seasoning oil is leached for 72 hours, and is considered to be caused by the residual impurities in the pepper melting into the oil, and the L value is obviously increased after the filtering and clarification, and is 11.88. The oxidation of fat is shown to be in positive correlation with the generation of yellow pigment, and the b value shows a trend that the b value rises firstly and then falls and then slowly rises in the processing process of the pepper flavoring oil as shown in table 1, and the trend is consistent with the change trend of the peroxide value. In the whole leaching process, the a value of the pepper seasoning oil is in a descending trend, which shows that the pigment in the pepper is gradually dissolved out along with the increase of the leaching time, and the a value difference between 24h and 72h of leaching is not obvious (P is less than 0.05), so that the color and luster of the pepper seasoning oil are not greatly influenced by longer leaching time.
TABLE 1 changes in color during processing of Zanthoxylum bungeanum seasoning oil
Note: l values represent light and shade, a values represent red and green, and b values represent yellow and blue; "+" indicates lighter, red, yellow, and "-" indicates darker, green, blue.
2. Influence of processing procedure on acid value of pepper seasoning oil
The oil and fat can generate a special and pungent odor 'rancid odor' after being reacted with oxygen, so that the quality of the oil and fat is reduced, and the content of free fatty acid in the oil and fat determines the quality of the oil and fat. The acid value is measured by the free fatty acid generated by triglyceride hydrolysis, and is considered as one of the main indexes for identifying the quality of the grease. The change of acid value in the processing process of the zanthoxylum bungeanum seasoning oil is shown in figure 2.
As can be seen from figure 2, the value of the pepper seasoning oil is obviously increased after 24 hours of extraction, probably because the moisture in the pepper accelerates the oxidation of oil and fat in the extraction process. The fluctuation range of the acid value of the sample in the processing processes of leaching for 24 hours, leaching for 72 hours, filtering, clarifying, finished products and the like is small and stable, the presumption is that moisture in the pepper is volatilized in the high-temperature leaching process, the moisture content in the grease is small at the moment, the stability of the grease is increased, the acid value after filtering is slightly improved, and the condition that residual trace moisture in the pepper is extruded during plate-and-frame filtering is considered. Therefore, the moisture content of the pepper should be strictly controlled in advance of pepper soaking so as to reduce the influence of the moisture of the pepper on the acid value in the processing process. The detection proves that the acid value of the finished product of the pepper seasoning oil is 0.3418mg/g, which is lower than the limit value 3mg/g specified in GB2716-2018, and meets the standard.
3. Influence of processing procedure on peroxide value of pepper seasoning oil
After the oil is oxidized, the taste and nutrition are influenced, and simultaneously, the biological activity of the oxidized oil is changed, so that the oxidized oil has certain damage effect on tissues and organs. The peroxide value is an important index for identifying the deterioration degree of the grease. The change of peroxide value in the processing process of the pepper seasoning oil is shown in figure 3.
As can be seen from FIG. 3, the crude oil peroxide value is 0.079g/100g, and the peroxide value is increased and decreased during the leaching process. The peroxide value is supposed to be increased when the soybean oil is leached for 24 hours, and the higher temperature catalyzes the oxidation of the grease in the heating process of the soybean oil; the peroxide value is reduced when leaching is carried out for 72 hours, and the peroxide is oxidized into aldehyde, ketone, acid and other small molecules, so that the peroxide value is reduced. The peroxide value is in the rising trend in the processing processes of filtering, clarifying and the like. The detection proves that the peroxide value of the finished product of the pepper seasoning oil is 0.089mg/g and is lower than the limit value of 0.25g/100g specified in GB2716-2018, and the pepper seasoning oil meets the national standard.
4. Influence of processing procedure on Zanthoxylum bungeanum Maxim amide
The Zanthoxylum amides are mostly chain unsaturated fatty acid amides, which are important flavor development substances (numb taste) in Zanthoxylum oil, and the high content of the Zanthoxylum amides include hydroxy-alpha-sanshool, hydroxy-beta-sanshool, hydroxy-gamma-sanshool, etc. The content change of hydroxy-beta-sanshool in the processing process of the zanthoxylum flavoring oil is shown in figure 4.
As can be seen from FIG. 4, the highest content of hydroxy-beta-sanshool in the pepper seasoning oil during the processing is 3.65mg/g, the lowest content is 2.62mg/g, which both exceed the standard 2.0mg/g of amide substances (calculated by hydroxy-beta-sanshool) in the pepper seasoning oil in the local standard of Sichuan province. Compared with the extraction for 24 hours, the content of the Zanthoxylum bungeanum amide is reduced during the extraction for 72 hours, and the Zanthoxylum bungeanum amide is possibly lost due to longer extraction time. Therefore, the leaching time in the later leaching period is not in direct proportion to the content of the Zanthoxylum piperitum amide in the flavoring oil, so that the leaching time can be properly shortened in the processing process to improve the production efficiency of enterprises. The content of the hydroxyl-beta-sanshool tends to be stable after the content of the hydroxyl-beta-sanshool is reduced in the later processing period of the seasoning oil, and the result of mutual transformation among isomers such as the hydroxyl-alpha-sanshool, the hydroxyl-beta-sanshool and the hydroxyl-gamma-sanshool is probably the result.
5. Influence of processing procedure on fatty acid of pepper seasoning oil
The fatty acid composition changes during the processing of zanthoxylum bungeanum seasoning oil are shown in table 2. As shown in Table 2, the content of unsaturated fatty acid in soybean oil is 84.6%, wherein the contents of linoleic acid and alpha-linolenic acid are 55.22% and 8.42% respectively. The difference between the fatty acid composition in the extraction (24 h), the extraction (72 h), the filtration, the clarification and the finished product zanthoxylum oil and the fatty acid composition in the crude oil is very small, which indicates that the glyceride in the zanthoxylum bungeanum maxim cannot be well dissolved in the soybean oil in the processing process of the zanthoxylum bungeanum maxim flavoring oil, and the result is consistent with the research result of Li Jin [7 ]. The fatty acid composition can not be used as an important index for controlling the quality in the processing process of the pepper seasoning oil.
TABLE 2 fatty acid composition changes during processing of Zanthoxylum bungeanum flavoring oil
The main components of the volatile flavor substances of the samples are analyzed, and the specific analysis results are as follows:
1. PCA analysis
An analysis chart of the main components among the samples in the processing process of the zanthoxylum bungeanum seasoning oil is shown in fig. 5. As can be seen from FIG. 5, the variance contribution rate of the first principal component is 90.083%, the variance contribution rate of the second principal component is 8.299%, and the cumulative total contribution rate of the first principal component and the second principal component is 98.382%, which indicates that the atlas can better reflect the integrity of the odor data in the measured sample. When the identification index is between 80 and 100, it indicates an effective data discrimination effect, and as can be seen from fig. 5, the identification index between samples is 95, indicating that the discrimination between samples is effective. No cross-over portion existed between 6 samples in the process of processing the pepper flavoring oil, which shows that 6 samples can be well separated by Heracles II ultra-fast gas-phase electronic nose. In the PCA analysis chart, the distance between the samples is in positive correlation with the odor difference among the samples, and as can be seen from the chart 5, a certain distance exists among the samples in the processing process of the pepper seasoning oil, which indicates that the odor difference among the samples is obvious, and the loss of flavor development substances in the processes of filtering, clarifying, filling and the like is considered. The processing time of each processing procedure of the pepper seasoning oil can be properly shortened, the flavor loss is reduced, and the production efficiency of enterprises is improved.
2. Discriminative index analysis
The distinguishing index is calculated based on the relative distance between the gravity centers of the two sample groups in the PCA chart, and the larger the distance between the two sample groups is, the smaller the difference in the groups is, the closer the distinguishing index is to 100 percent, namely, the distinguishing index is positively correlated with the difference between the samples. The index of distinction between samples during the processing of zanthoxylum bungeanum seasoning oil is shown in table 3. As can be seen from table 3, the discrimination indexes between the samples are large, indicating that the difference between the samples is large.
TABLE 3 analysis of the index of distinctiveness between samples during the processing of zanthoxylum bungeanum seasoning oil
Note: YY: crude oil; JT-24: leaching (24 h); JT-72: leaching (72 h); GL: filtering; CQ: clarifying; and (3) CP: finished product
3. Influence of processing procedure on volatile flavor substances of pepper seasoning oil
The volatile flavor substances of the sample in the processing process of the pepper seasoning oil are measured by using a Heracles II ultra-fast gas-phase electronic nose, and the volatile flavor components possibly contained in the sample are obtained by combining with a retrieval database (see Table 4). As can be seen from Table 4, the difference in flavor components between soybean oil and zanthoxylum seasoning oil is large, wherein hexanal, nonanal, heptanal, (E, E) -2,4-heptadienal are characteristic flavor substances in soybean oil. The types of flavor substances possibly contained in samples of the pepper seasoning oil among processing procedures are basically consistent, and the pepper seasoning oil comprises alkanes, ketones, aldehydes, esters, olefins, alcohols and the like, wherein the alpha-terpineol has obvious antibacterial and anti-inflammatory effects; linalool is an important flavoring substance with numb taste of pepper, has the effects of oxidation resistance, hypnosis and the like, and is widely applied to the flavoring industry. The threshold values of various volatile flavor substances are different, such as ketone and alcohol compounds with higher threshold values and aldehyde and pyrazine compounds with lower threshold values, so that small changes of the content of the volatile flavor substances can cause great influence on the whole smell, which can also be the reason of the smell difference among samples in the processing procedure.
TABLE 4 qualitative analysis of aroma components of samples during processing of zanthoxylum bungeanum seasoning oil
Note: YY: crude oil; JT-24: leaching (24 h); JT-72: leaching (72 h); GL: filtering; CQ: clarifying; and (3) CP: finished product
In conclusion, experiments are carried out on the physical and chemical indexes and the volatile flavor substance change in the processing process of the pepper seasoning oil. The a value difference in the extraction process of the zanthoxylum flavoring oil is not obvious. The acid value is in the overall rising trend, and the peroxide value and the Zanthoxylum bungeanum amide are in the trend of rising first and then decreasing. The fatty acid composition is almost not different among the procedures in the processing process, so the fatty acid composition cannot be used as an important index for controlling the quality in the processing process of the pepper seasoning oil. The odor difference among samples in each procedure in the processing process of the pepper seasoning oil is obvious, 8 possible volatile flavor substances are detected in the soybean oil, wherein the main volatile flavor substances are hexanal, nonanal, heptanal, (E, E) -2,4-heptadienal, and the 13 possible volatile flavor substances are detected in the pepper seasoning oil, and the main volatile flavor substances are alcohols and olefins. During the processing of the pepper seasoning oil, the moisture content of the raw materials is further controlled to reduce the influence of moisture in pepper on the acid value; the overlong leaching time has no positive effect on the color and luster and the content of the Zanthoxylum bungeanum amide, and volatile flavor substances in the Zanthoxylum bungeanum seasoning oil are lost in the processing process, so that enterprises can consider properly reducing the leaching time during processing, shorten the time of each processing procedure to reduce the flavor loss, and improve the production efficiency of the enterprises.
Although the embodiments of the present invention have been disclosed for illustrative purposes, those skilled in the art will appreciate that: various substitutions, changes and modifications are possible without departing from the spirit and scope of the invention and the appended claims, and therefore the scope of the invention is not limited to the embodiments disclosed.
Claims (8)
1. A method for detecting volatile flavor substances in spice oil based on PCA analysis technology is characterized by comprising the following steps: the method comprises the following steps:
(1) Spice oil sample preparation
Heating raw oil to 180 ℃, pouring the raw oil into an extraction tank filled with carefully selected and crushed spices, stirring the raw oil once every 5min by using a stirring rod for 30min, soaking the raw oil in the extraction tank for 3-4 days to ensure that the spices are fully extracted, filtering an upper oil sample by using a plate type closed filter after soaking, and clarifying the filtered oil sample in a storage tank to obtain a final finished oil sample;
(2) Performing index measurement and volatile flavor substance measurement on the spice oil sample, wherein Heracles II ultra-fast gas phase electronic nose is selected for detection in the volatile flavor substance measurement;
(3) Carrying out statistical analysis on the measurement data of the volatile flavor substances by using a PCA (principal component analysis) method;
(4) And (3) analyzing the distinguishing index, wherein the distinguishing index is calculated based on the relative distance between the gravity centers of the two sample groups in the PCA diagram, the larger the distance between the two sample groups is, the smaller the difference in the groups is, and the closer the distinguishing index is to 100 percent, namely, the distinguishing index is positively correlated with the difference between the samples.
2. The method for detecting volatile flavor substances in spice oil based on PCA analysis technology as claimed in claim 1, wherein the method comprises the following steps: and (3) carrying out index measurement on the spice oil sample in the step (2), wherein the index measurement comprises the following steps: amide compound determination, color determination, acid value determination, peroxide value determination and fatty acid determination.
3. The method for detecting volatile flavor substances in spice oil based on PCA analysis technology as claimed in claim 1, wherein the method comprises the following steps: the method for determining the amide compound comprises the following steps:
(1) Standard curve establishment
Taking 5mg of a hydroxy-beta-sanshool standard substance, diluting the volume to 5mL with methanol to obtain a hydroxy-beta-sanshool standard solution, respectively sucking 0mL, 1mL, 2mL, 3mL, 4mL, 5mL, 6mL, 7mL and 8mL of the standard solution, preparing a hydroxy-beta-sanshool solution with the concentration of 0-8 mu g/mL with methanol, measuring the absorbance at 267nm, and drawing a standard curve by taking the concentration as a horizontal coordinate and the absorbance value as a vertical coordinate;
(2) Zanthoxylum bungeanum amide determination
Measuring the content of the Zanthoxylum bungeanum amide by referring to a method in appendix A of DBS51/008-2019 food safety local standard Zanthoxylum oil, calculating the content of the hydroxyl-beta-sanshool according to a standard curve, wherein a regression equation is y =0.1501x-0.1288 2 =0.9983 where y is absorbance value and x is zanthoxylum amid content.
4. The method for detecting volatile flavor substances in spice oil based on PCA analysis technology as claimed in claim 1, wherein the method comprises the following steps: and (3) detecting volatile flavor substances in the step (2) by using a Heracles II ultra-fast gas-phase electronic nose, wherein the detection method comprises the steps of taking 2g of spice oil samples into a 20mL headspace bottle, preheating the spice oil samples in a water bath kettle at 55 ℃ for 24min, manually injecting samples, and paralleling 3 samples.
5. The method for detecting volatile flavor substances in spice oil based on PCA analysis technology as claimed in claim 1 or 4, wherein the method comprises the following steps: detecting parameters: the sample inlet temperature is 200 ℃, the sample volume is 5000 mu L, the injection speed is 125 mu L/s, the sample introduction time is 45s, the trap initial temperature is 40 ℃, the shunt rate is 10mL/min, the final temperature is 200 ℃, the initial column temperature is 50 ℃, the temperature is increased to 80 ℃ at 1 ℃/s, then the temperature is increased to 250 ℃ at 3 ℃/s, the collection time is 110s, and the FID detector temperature is 260 ℃.
6. A spice oil volatile flavor substance detection method based on PCA analysis technology is applied to vegetable zanthoxylum oil, and PCA analysis is respectively carried out on crude oil before extraction, an oil sample after 24 hours of extraction, an oil sample after 72 hours of extraction, a plate-frame filtration oil sample, a clarified oil sample and finished oil.
7. The use of a method for detecting the volatile flavor substances in spice oil based on PCA analysis technology as claimed in claim 6, wherein the method comprises the following steps: the PCA method is applied to the processing process of the pepper seasoning oil in the vegetable pepper oil, the odor difference among samples in each process is obvious, 8 volatile flavor substances including hexanal, nonanal, heptanal, (E, E) -2,4-heptadienal are detected in the soybean oil, and 13 volatile flavor substances including alcohols and olefins are detected in the pepper seasoning oil.
8. The use of a method for detecting the volatile flavor substances in spice oil based on PCA analysis technology as claimed in claim 6, wherein the method comprises the following steps: the PCA method analysis shows that the variance contribution rate of the first principal component is 90.083%, the variance contribution rate of the second principal component is 8.299%, the cumulative total contribution rate of the first principal component and the second principal component is 98.382%, the identification index among samples is 95, and the distance among the samples in a PCA analysis chart is in positive correlation with the odor difference among the samples.
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