• 专利附录
  • 专利说明
  • 权利要求
  • 类似技术
  • 同族专利
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    • 专利摘要:
    The present invention discloses a identification method of characteristic volatile compounds in meat or meat products, including: extracting volatile compounds from meat or meat products and detecting each component concentration; calculating odor activity value and contribution rate of each component; selecting N components whose cumulative contribution rate and odor activity value is respectively greater than preset value a and b, preparing a recombination model 1 of N components standard sample and odorless meat or meat products material, deleting one of N components, and preparing a recombination model 2 with odorless meat or meat products materials, comparing flavor of recombination model 1 with 2, wherein component caused difference in flavor is characteristic volatile compound of meat or meat products. The present invention can avoid inaccurate drawback of traditional method by single gas chromatography-olfactometry-mass spectrometry, and can accurately and quickly identify volatile compounds of meat or meat products,
    公开号:NL2022959A
    申请号:NL2022959
    申请日:2019-04-17
    公开日:2019-05-29
    发明作者:Zhang Dequan；Liu Huan；Wang Zhenyu；Chen Li；Pan Teng；Li Xin；Hui Teng；Hou Chengli；Zheng Xiaochun
    申请人:Institute Of Food Science And Tech Chinese Academy Of Agricultural Sciences；
    IPC主号:
    专利说明:

    IDENTIFICATION METHOD OF CHARACTERISTIC VOLATILE COMPOUNDS IN MEAT OR MEAT PRODUCTS TECHNICAL FIELD
    [0001] The present invention relates to the field of food inspection technology. More specifically, the present invention relates to an identification method of characteristic volatile compounds in meat or meat products.
    BACKGROUND
    [0002] Traditional meat products are Chinese business cards and treasure of Chinese diet culture, especially barbecue, pot-stewed and cured products. Traditional meat products have unique and rich flavors, which are popular among consumers, and their flavor and volatile compounds are related. The determination of volatile compound is not only related to its content, but also closely related to its extraction and analysis methods. The traditional method for identifying characteristic volatile compounds contains quantitative analysis combined with gas chromatography-mass spectrometry, and determination of odor activity value. The above traditional method has certain drawbacks. Gas chromatography-mass spectrometry is only used to clarify the components of the volatile compounds and their relative contents, and lacks subjective sensory evaluation. The accuracy of the volatile compounds by determination of odor activity value is not enough and further verification is lacking. For example, such as the odor activity value of 2-methylbutanal is greater than 1, but this compound does not contribute significantly to the overall flavor of the meat or meat products. Accordingly, a rapid and accurate method for identifying characteristic volatile compounds in meat or meat products is needed in this field.
    DESCRIPTION
    [0003] A purpose of the present invention is to solve at least above problems, and to provide, at least, the advantages that will be described later.
    [0004] Another purpose of the present invention is to provide an identification method of characteristic volatile compounds in meat or meat products, which uses headspace solid phase microextraction combined with gas chromatography-olfactometry-mass spectrometry to detect volatile compounds in meat or meat products. The volatile compounds in meat or meat products are analyzed by contribution rate and cumulative contribution rate method, and the characteristic volatile compounds are identified by recombination model, thereby solving the problem that identification method of characteristic volatile compounds in the prior art is not accurate.
    [0005] In view of purposes mentioned above and other advantages, the present invention provides an identification method of characteristic volatile compounds in meat or meat products, including the following steps: [0006] step one, extracting volatile compounds from meat or meat products and detecting concentration of each component in volatile compounds; [0007] step two, calculating odor activity value of each component, and obtaining contribution rate of each component according to the ratio of the odor activity value of each component to sum of odor activity value of all components; [0008] step three, sorting the contribution rate of each component in descending order, selecting M components whose cumulative contribution rate is greater than preset value a in the descending order, and then selecting N components whose odor activity value is greater than preset value b from the M components having cumulative contribution rate greater than preset value a; [0009] step four, preparing odorless meat or meat products material, preparing a mixed standard solution 1 of the N components obtained in the step three according to the concentration of each component in the step one, adding the mixed standard solution 1 into the odorless meat or meat products material to form a recombination model 1, deleting one of the N components obtained in the step three, preparing a mixed standard solution 2 of remaining components according to the concentration of each component in the step one, adding the mixed standard solution 2 into the odorless meat or meat products materials to form a recombination model 2, comparing flavor of the recombination model 1 with the recombination model 2, wherein volatile compound that causes difference in flavor is characteristic volatile flavor substance of meat or meat products.
    [00010] Preferably, apparatus for detecting volatile compounds is a gas chromatography-olfactometry-mass spectrometry, wherein heating process of the gas chromatography-olfactometry-mass spectrometry is: initial column temperature Ti °C, keeping ti min, heating to T2 °C at a rate of vi °C/min, heating to T3 °C at a rate of Y2 °C/min, heating to T4 °C at a rate of v °C/min, and keeping ti min, wherein Ti is smaller than or equal to 40, ti is greater than or equal to 3, T2 is greater than or equal to 60 and smaller than or equal to 80, T3 is greater than or equal to 120 and smaller than or equal to 140, T4 is greater than or equal to 230, t2 is greater than or equal to 3, and vi is greater than vi and smaller than v ,.
    [00011] Preferably, the extraction method of volatile compounds from meat or meat products is a headspace solid phase microextraction method, and the extraction process comprises: weighing meat or meat products, adding saturated sodium chloride solution to meat or meat products in a ratio of 1 mL : 1 g, adding a standard of organic compound, stirring, preheating at 40-60 °C for 8-15 min, and adsorbing by CAR/PDMS extraction fiber at 40-60 °C for 40-60 min [00012] Preferably, the process of qualitatively detecting volatile compounds by the gas chromatography-olfactometry-mass spectrometry includes: retrieving by a mass spectrometry library, calculating retention index, analyzing by sniffer, and performing standard qualitative analysis to obtain specific components of volatile compounds.
    [00013] Preferably, the process of quantitatively detecting the concentration of each component in volatile compounds by the gas chromatography-olfactometry-mass spectrometry includes: preparing a plurality of odorless meat or meat products materials, detecting each component in volatile compounds by the gas chromatography-olfactometry-mass spectrometry, taking standard to prepare mixed standard solution 3 with different concentration, adding the mixed standard solution 3 into a plurality of odorless meat or meat products materials, extracting volatile compounds of each meat or meat products material containing the mixed standard solution 3 by headspace solid phase microextraction, detecting peak area of characteristic ion fragments of each component by the gas chromatography-olfactometry-mass spectrometry, establishing a standard curve equation between the peak area of characteristic ion fragments and the concentration of each component in volatile compounds, and determining the concentration of each component in volatile compounds of meat or meat products according to the peak area of characteristic ion fragments of each component in volatile compounds of meat or meat products by the gas chromatography-olfactometry-mass spectrometry.
    [00014] Preferably, preparation method of odorless meat or meat products material includes: weighing meat or meat products, mixing the meat or meat products, diethyl ether and n-pentane in a ratio of 1 g : 2 mL : 1 mL, shaking in a shaker, filtering, removing organic solution, repeating operation several times until the meat or meat products are odorless, freeze-drying odorless meat or meat products, and adding purified water is added, wherein amount of the purified water is consistent with water content of the meat or meat products.
    [00015] Preferably, method for comparing flavor of the recombination model 1 with the recombination model 2 is sensory triangular test.
    [00016] Preferably, the preset value a is 90%, and the preset value b is 1.
    [00017] Preferably, capillary column of the gas chromatography-olfactometry-mass spectrometry is DB-Wax, and the heating process includes: keeping at initial column temperature 40 °C for 3 min, heating to 70 °C at a rate of 2 °C/min, heating to 130 °C at a rate of 3 °C/min, heating to 230 °C at a rate of 10 °C/min, and keeping 10 min.
    [00018] Preferably, the process for extracting volatile compounds from meat or meat products includes: weighing meat or meat products, adding saturated sodium chloride solution to the meat or meat products in a ratio of 1 mL : 1 g, adding 2-methyl-3-heptanone standard, placing a magnetic rotor, performing magnetic stirring, preheating at 55 °C for 10 min, and finally adsorbing by a 75 pm CAR/PDMS extraction fiber at 55 °C for 45 min.
    [00019] The present invention includes at least the following advantages: [00020] First, the contribution rate method used in the present invention can initially obtain volatile compounds having a large contribution rate of meat or meat products, and the cumulative contribution rate method can determine volatile compounds having a larger contribution rate of meat or meat products.
    [00021] Second, Combination of detecting and recombination model used in the present invention can avoid inaccurate drawback of traditional method by single gas chromatography-olfactometry-mass spectrometry, and the present invention can accurately identify volatile compounds of meat or meat products, and have high accuracy rate.
    [00022] Third, the heating process of the gas chromatography-olfactometry-mass spectrometry is deeply optimized in the present invention, so that types and contents of volatile compounds detected are significantly increased, and extraction effect of volatile compounds is improved.
    [00023] Fourth, meat or meat products in the present invention are added a saturated sodium chloride solution, and stirred with a magnetic stirring device to better release volatile compounds, by which the content of volatile compounds is significantly increased, and the extraction effect of volatile compounds is improved. The 2-methyl-3-heptanone standard sample is used as an internal standard substance, which is more suitable for extraction of volatile compounds in meat or meat products, so that detection accuracy of volatile compounds is greatly improved.
    [00024] Other advantages, objects, and features of the present invention will be showed in part through following description, and in part will be understood by those skilled in the art from study and practice of the present invention.
    BRIEF DESCRIPTION OF THE DRAWINGS
    [00025] Fig. 1 is a chromatogram of volatile compounds in meat or meat products according to an embodiment of the present invention.
    [00026] Fig. 2 is a chromatogram of volatile compounds in meat or meat products according to comparative example 2 of the present invention.
    [00027] Fig. 3 is a chromatogram of volatile compounds in meat or meat products according to comparative example 3 of the present invention.
    [00028] Fig. 4 is a standard curve and standard curve equation of l-octene-3-ol in volatile compounds according to the embodiment of the present invention.
    [00029] Fig. 5 is a standard curve and standard curve equation of nonanal in volatile compounds according to the embodiment of the present invention.
    [00030] Fig. 6 is a standard curve and standard curve equation of dimethyltrisulfide in volatile compounds according to the embodiment of the present invention.
    [00031] Fig. 7 is a standard curve and standard curve equation of guaiacol in volatile compounds according to the embodiment of the present invention.
    [00032] Fig. 8 is a thermal image of odor activity value of components having a cumulative contribution rate greater than 90% and a odor activity value greater than 1 in volatile compounds according to the embodiment of the present invention.
    [00033] Fig. 9 is a thermal image of contribution rate of components having a cumulative contribution rate greater than 90% and a odor activity value greater than 1 in volatile compounds according to the embodiment of the present invention.
    [00034] Fig. 10 is a thermal image of odor activity value of 9 components having a cumulative contribution rate greater than 90% and a odor activity value greater than 1 in volatile compounds according to the embodiment of the present invention.
    [00035] Fig. 11 is a diagram showing flavor characteristics of characteristic volatile compounds according to the embodiment of the present invention.
    DETAILED DESCRIPTION
    [00036] The present invention will now be described in further detail with reference to the accompanying drawings in order to enable person skilled in the art to practice with reference to the description.
    [00037] It should be noted that experimental methods described in the following embodiments are all conventional methods unless otherwise specified, and reagents and materials are commercially available unless otherwise specified. It should be noted that in the description of the present invention, the terms of "transverse ", "longitudinal ", "up", "down", "front", "behind", "left", "right", "vertical", "horizontal", "top", "bottom", "inner", "outer" and the like are based on the orientation or positional relationship shown in the drawings for convenience of describing the present invention and simplifying description. It is not intended or implied that the device or element must have a particular orientation and be constructed and operated in a particular orientation, and therefore it should not be construed as limiting the present invention.
    [00038] Embodiment [00039] Specific flow of the embodiment will only be described below, hi fact, inventors have identified samples of different brands of meat products by the following embodiment.
    [00040] step one, weighing 4 g of meat (duck breast skin or duck breast) in a 20 mL sample vial, adding 4 mL of saturated sodium chloride solution, adding 1.5 pL of 2-methyl-3-heptanone, performing magnetic stirring, preheating at 55 °C for 10 min, and finally adsorbing at 55 °C for 45 min through a 75 pm CAR/PDMS extraction fiber.
    [00041] step two, taking out of the extraction fiber, quickly inserting into an inlet of a gas chromatography-olfactometry-mass spectrometry, and then starting the gas chromatography-olfactometry-mass spectrometry to collect data, wherein capillary column of the gas chromatography-sniffer-mass spectrometry was DB-Wax (30 m * 320 pm x 0.25 pm) and uses non-diversion mode injection, flow rate of carrier gas (He) was 1.0 mL / min, temperature of the sniffer was 230 °C, and the heating process included: keeping at initial column temperature 40 °C for 3 min, heating to 70 °C at a rate of 2 °C/min, heating to 130 °C at a rate of 3 °C/min, heating to 230 °C at a rate of 10 °C/min, and keeping 10 min.
    [00042] Mass spectrometry conditions: ionization energy. El; scanning range m/z: 50-500; ion source temperature: 230 °C; scanning frequency: 1.7 times / sec.
    [00043] The chromatogram of obtained volatile compounds was shown as Fig. 1.
    [00044] Qualitative analysis of volatile compounds: [00045] (1) retrieving by a mass spectrometry library: experimental data processing was performed by the Agilent Masshunter Qualitative Analysis software system. The computer search of unknown compounds was matched with the NIST MS 2.0 library, and identification result was only reported when positive and negative matching degrees were greater than 800 (maximum value was 1000).
    [00046] (2) calculating retention index: the same heating process as in the step two was used, 2-methyl-3-heptanone was used as a standard, the retention index of volatile compounds in meat or meat products were calculated by retention time, and retention index (RI) of compounds in referred literature was compared with the retention index of volatile compounds in meat or meat products.
    [00047] Formula for calculating the retention index RI was: RI = 100η + 100(tx - tn) / (tn+i - tn), wherein n was the number of carbon, tx, tn and tn+i were respectively peak time of unknown volatile flavor substance, Cnand Cn+i, and tx was greater than tn and less than tn+i [00048] (3) analyzing by the sniffer: volatile compounds separated by the gas chromatography were entered into a mass spectrometry detector and the sniffer in a ratio of 1:1. A sensory evaluator sniffs and records the characteristics and intensity of volatile compounds. On this basis, sniffing results was compared with flavor characteristics of the standard of substance, [00049] (4) performing qualitative analysis of the standard sample: using mixed standard of the standards of volatile compounds as an external standard, detecting according to GC-MS heating process of sample, comparing and analyzing the peak time of the standard sample and the peak time of the volatile compounds.
    [00050] Components of volatile compounds determined by combination of mass spectrometry library, retention index calculation, sniffer analysis and qualitative analysis of the standards contained 42 kinds of volatile compounds, including aldehydes and sulfur-containing compounds, alcohols, ketones, phenols, acids and nitrogen-containing compounds, wherein aldehydes (16 species) are mainly pentanal, hexanal, (£, £)-2,4-decadienal etc., sulfur-containing compounds (3 species) are dimethyl trisulfide, 2-furfurylthiolandmethional.
    [00051] Quantitative analysis of volatile compounds: [00052] (1) preparation method of odorless meat or meat products material included: weighing meat or meat products, mixing the meat or meat products, diethyl ether and n-pentane in a ratio of 1 g : 2 mL : 1 mL, shaking in a shaker for 8 h, filtering for removing organic solution, repeating operation several times until the meat or meat products was odorless, freeze-drying odorless meat or meat products for 12 h, and adding purified water was added, wherein amount of the purified water was consistent with water content of the meat or meat products, and the water content of the meat or meat products was determined by the quality difference of samples before and after freeze-drying.
    [00053] (2) each component of volatile compounds detected by the gas chromatography-olfactometry-mass spectrometry was prepared as a standard solution of 10 mg/g by methanol (wherein the standard solution contained all components of volatile compounds, and each component had a concentration of 10 mg/g). The standard solution was then diluted to a mixed standard solution 3 with different concentrations (eg 1 mg/g, 500 ng/g, 250 ng/g, 100 ng/g, 50 ng/g, 25 ng/g, 10 ng/g, 5 ng/ and 1 ng/g, etc.), and the mixed standard solution 3 with different concentrations was added into a plurality of odorless meat or meat products materials, extracting volatile compounds of each meat or meat products material containing the mixed standard solution 3 by headspace solid phase microextraction, detecting peak area of characteristic ion fragments of each component by the gas chromatography-olfactometry-mass spectrometry, establishing a standard curve equation between the peak area of characteristic ion fragments and the concentration of each component in volatile compounds, and determining the concentration of each component in volatile compounds of meat or meat products according to the peak area of characteristic ion fragments of each component in volatile compounds of meat or meat products by the gas chromatography-olfactometry-mass spectrometry.
    [00054] Since there were many components of volatile compounds, standard curves and standard curve equations of the four components of l-octene-3-ol, nonanal, dimethyl trisulfide and guaiacol and their standard curve equations were only described below, as shown in Fig. 4-7.
    [00055] The standard curve equation of l-octene-3-ol was y=3 X 10°x-19.883, wherein correlation coefficient R2 was 0.9937.
    [00056] The standard curve equation of nonanal was y=8X 10'5x-358.28, wherein correlation coefficient R2 was 0.9923.
    [00057] The standard curve equation of dimethyltrisulfide was y=3 X 10^-6.4727, wherein correlation coefficient R2 was 0.9998.
    [00058] The standard curve equation of guaiacol was y=2X 10^-6.8828, wherein correlation coefficient R2 was 0.9961.
    [00059] Step three, analysis of contribution rate of each component in volatile compounds: odor activity value of each component was calculated by ratio of the concentration of each component to the threshold (the threshold of each component was referred through relevant literature: ZHU J, CHEN F, WANG L, et al. Characterization of the Key Aroma Volatile Compounds in Cranberry (Vaccinium macrocarpon Ait) Using Gas Chromatography-Olfactometry (GC-O) and Odor Activity Value (OAV)[J]_ Journal of Agricultural and Food Chemistry, 2016, 64 (24):4990-4999. DOI: 10.1021/acs.jafc.6b01150; GEMERT, L. J. V, Compilations of odour threshold values in air, water and other media. 2003; KERLER J, GROSCH W. Character impact odorants of boiled chicken: changes during refrigerated storage and reheating[J], Zeitschrift fuer Lebensmittel-Untersuchung und -Forschung A, 1997, 205(3):232-238. DOI: 10.1007/s002170050157; CZERNY M, CHRISTLBAUER M, CHRISTLBAUER M, et al. Re-investigation on odour thresholds of key food aroma compounds and development of an aroma language based on odour qualities of defined aqueous odorant solutions[J], European Food Research and Technology, 2008, 228(2):265-273. DOI: 10.1007/s00217-008-0931-x; GREGER V, SCHIEBERLE P. Characterization of the key aroma compounds in apricots (Prunus armeniaca) by application of the molecular sensory science concept[J], Journal of Agricultural & Food Chemistry, 2007, 55(13):5221-5228. DOI: 10.102 l/jf0705015 ; CHRISTLBAUER M, SCHIEBERLE P. Evaluation of the key aroma compounds in beef and pork vegetable gravies a la chef by stable isotope dilution assays and aroma recombination experiments [J], Journal of Agricultural & Food Chemistry, 2011, 59(24):13122-13130. DOI: 10.1021/jf203340a, etc.), the contribution ratio of each component was obtained according to the ratio of odor activity value of the single component to the sum of odor activity values of all components, and compound with larger contribution rate was more important.
    [00060] Step 4: Analysis of cumulative contribution rate of each component in volatile compounds: the contribution rate of each component was sorted in order of largest to smallest, and components having a cumulative contribution rate greater than 90% were selected in descending order, and components having an odor activity value greater than 1 were selected from the components having a cumulative contribution rate greater than 90%.
    [00061] As shown in Fig. 1, inventors listed contribution rate and cumulative contribution rate of volatile compounds of some branded roast duck meat samples having a cumulative contribution rate greater than 90% and an odor activity value greater than 1.
    [00062] Table 1 [00063]
    [00064] Step five, preparing odorless meat or meat products material (method was the same as above), preparing a mixed standard solution 1 of the 18 components obtained in the step four according to the concentration of each component in the step one (the mixed standard solution contained the 18 components, and the concentration of each component was the same as that detected in the step two), adding the mixed standard solution 1 into the odorless meat or meat products material to form a recombination model 1, deleting one of the 18 components obtained in the step four, preparing a mixed standard solution 2 of remaining components according to the concentration of each component in the step one, adding the mixed standard solution 2 into the odorless meat or meat products materials to form a recombination model 2, comparing flavor of the recombination model 1 with the recombination model 2, wherein method for comparing flavor of the recombination model 1 with the recombination model 2 was sensory triangular test, and volatile compound that caused difference in flavor was characteristic volatile compound of meat or meat products. If component that did
    not cause difference in flavor was removed, and component that caused difference in flavor was retained, a recombinant model 3 was continued to prepare. If the flavor of the recombinant model 3 is basically same as the flavor of meat or meat products, the retained component was characteristic volatile compound of all meat or meat products, and then analyzing to determine flavor characteristics of meat or meat products, as shown in Fig. 11.
    [00065] Comparative example 1 [00066] step one and step two were the same as that of the embodiment, and there were no step three, step four, and step five.
    [00067] Comparative example 2 [00068] step one was the same as that of the embodiment [00069] step two, taking out of the extraction fiber, quickly inserting into an inlet of a gas chromatography-olfactometry-mass spectrometry, and then starting the gas chromatography-olfactometry-mass spectrometry to collect data, wherein capillary column of the gas chromatography-olfactometry-mass spectrometry was HP-5MS (30 m x 0.25 mm x 0.25 pm) and uses non-diversion mode injection, flow rate of carrier gas (He) was 1.0 mL / min, temperature of the sniffer was 230 °C, and the heating process included: keeping at initial column temperature 40 °C for 3 min, heating to 70 °C at a rate of 3 °C/min, heating to 180 °C at a rate of 5 °C/min, heating to 230 °C at a rate of 10 °C/min, and keeping 5 min.
    [00070] Mass spectrometry conditions, qualitative analysis of volatile compounds, quantitative analysis of volatile compounds and odor activity value were the same as those in the embodiment.
    [00071] The chromatogram of obtained volatile compounds was shown in Fig. 2.
    [00072] Comparative example 3 [00073] step one was the same as that of the embodiment [00074] step two, taking out of the extraction fiber, quickly inserting into an inlet of a gas chromatography-olfactometry-mass spectrometry, and then starting the gas chromatography-olfactometry-mass spectrometry to collect data, wherein capillary column of the gas chromatography-olfactometry-mass spectrometry was HP-5MS (30 m χ 0.25 mm χ 0.25 μηι) and uses non-diversion mode injection, flow rate of carrier gas (He) wasl.O mL / min, temperature of the sniffer was 230 °C, and the heating process included: keeping at initial column temperature 40 °C for 2 min, heating to 70 °C at a rate of 2 °C/min, heating to 130 °C at a rate of 3 °C/min, heating to 230 °C at a rate of 10 °C/min.
    [00075] Mass spectrometry conditions, qualitative analysis of volatile compounds, quantitative analysis of volatile compounds and odor activity value were the same as those in the embodiment.
    [00076] The chromatogram of obtained volatile compounds was shown in Fig. 3.
    [00077] Result analysis [00078] Chromatogram analysis [00079] As shown in Fig. 1, Fig. 2 and Fig. 3, various components of volatile compounds of the embodiment (Fig. 1) can be well separated, the chromatogram of the embodiment had not overlapping peaks and heavy-tailed phenomenon, and the number of peaks was large. The peak shape of various components in volatile compounds of comparative example 2 (Fig. 2) and comparative example 3 (Fig. 3) was not well separated, chromatograms had heavy overlapping peaks and heavy-tailed phenomenon, and the number of peaks was small. The above indicated that gas chromatography column polarity and heating process significantly affected analytical ability of volatile compounds in meat or meat products. A total of 42 volatile compounds were detected in the embodiments, including aldehydes and sulfur-containing compounds, alcohols, ketones, phenols, acids and nitrogen-containing compounds, wherein aldehydes (16 species) were mainly pentanal, hexanal, (E, £)-2,4-decadienal etc., sulfur-containing compounds (3 species) are dimethyl trisulfide, 2-furfurylthiol and methional. Volatile compounds detected in comparative example 2 and 3 were less than 30. Therefore, DB-Wax extraction method of volatile compounds in meat or meat product of the present invention was more effective than FIP-5MS extraction method (p < 0.05), and volatile compounds can be better separated by the heating process in the embodiment.
    [00080] (2) Comparative analysis of thermal image of odor activity values and thermal image of contribution rate [00081] Thermal image of odor activity values of components having a cumulative contribution rate greater than 90% and an odor activity value greater than 1 in volatile compounds of the embodiment (the darker the color, the larger the odor activity value) was shown in Fig.8.
    [00082] Thermal image of contribution rate of components having a cumulative contribution rate greater than 90% and a odor activity value greater than 1 in volatile compounds of the embodiment (the darker the color, the larger the contribution rate) was shown in Fig.9.
    [00083] Thermal image of odor activity value of components having a cumulative contribution rate greater than 90% and an odor activity value greater than 1 in volatile compounds of the embodiment was shown in Fig. 10.
    [00084] Comparison results of flavor characteristics and strength of characteristic volatile compounds obtained by the embodiment with those of meat or meat products were shown in Fig. 11.
    [00085] As shown in Fig. 8, Fig. 9 and Table 1, there were 18 kinds of components having a cumulative contribution rate greater than 90% and an odor activity value greater than 1 in volatile compounds, including 12 aldehydes, 3 sulfur-containing compounds and 1 alcohols. But it was difficult to find characteristic volatile compounds from Fig. 8. The odor activity value of each component in the volatile compounds was only calculated in the Comparative Example 1. Even if the odor activity value was greater than 1, components of volatile compounds in meat or meat products cannot be further analyzed. This was disadvantage of this method.
    [00086] The contribution rate was used to visualize explanation contribution of each component of volatile compounds in meat or meat products. As shown in Fig. 9, the volatile compound in meat or meat products were mainly 2-furfurylthiol and dimethyl trisulfide, followed by methional and (K, A)-2,4-decadienal. This demonstrated that the contribution rate method and the cumulative contribution rate method provided by the present invention can identify characteristic volatile compounds more intuitively.
    [00087] In order to more accurately determine components of characteristic volatile compounds in meat or meat products, the embodiment continued to compare different recombination models using a sensory triangular test, as shown in Fig. 10 and 11, components of characteristic volatile compounds in meat or meat products had 9 kinds, including 2-furfurylthiol, dimethyl trisulfide, methional, hexanal, heptanal, octanal, nonanal, (£,£')-2,4-decadienal and l-octen-3-ol. Characteristic flavors of meat or meat products were fatty flavor, roast flavor and meat flavor. Thus, the method provided by the present invention can accurately determine components of characteristic volatile compounds in meat or meat products as well as the characteristic flavors of the characteristic volatile compounds.
    [00088] Although embodiments of the present invention have been disclosed as above, they are not limited to the applications listed in the Specification and implementation modes. They can be applied to all kinds of fields suitable for the present invention. Additional modifications can be easily implemented for those who are familiar with the field. Therefore, the present invention is not limited to specific details and the legends shown and described herein without deviation from the general concepts confined in the Claim and the Equivalents.
    权利要求:
    Claims (10)
    [1]
    A method for identifying characteristic volatile compounds in meat or meat products, comprising the steps of: step 1: extracting volatile compounds from meat or meat products and detecting the concentration of each component in the volatile compounds; - step 2: calculating an odor activity value of each component, and obtaining a contribution rate of each component according to a ratio of the odor activity value of each component to the sum of the odor activity values of all components; - step 3: sorting the contribution rate of each component in descending order, selecting M components whose cumulative contribution rate is greater than a preset value a in descending order, and then selecting N components whose odor activity value is greater than a preset value b from the M components with the cumulative contribution rate greater than the preset value a; - step 4: preparing an odorless meat or meat product matrix, preparing a mixed standard solution 1 of the N components obtained in step 3 according to the concentration of each component in step 1, adding the mixed standard solution 1 to the odorless meat or meat product matrix to form a recombination model 1, removing one of the N components obtained in step 3, preparing a mixed standard solution 2 of the remaining components according to the concentration of each component in step 1, adding the mixed standard solution 2 to the odorless meat or meat product matrix to form a recombination model 2, comparing the taste of the recombination model 1 with the recombination model 2, wherein the volatile compound causing difference in odor is the characteristic volatile compound of meat or meat products.
    [2]
    A method for identifying characteristic volatile compounds in meat or meat products according to claim 1, characterized in that a device for detecting volatile compounds is a gas chromatography olfactometry mass spectrometry, wherein the heating process of the gas chromatography olfactometry mass spectrometry includes: maintaining at the initial column temperature of Ti ° C, Ti <40, for ti min, ti> 3, heating to T2 ° C at a rate of vi ° C / min, 60 <T2 <80, heating to Ti ° C with a speed of V2 ° C / min, 120 <T , <140, and then heating to Tt0C with a speed of V3 ° C / min, T *> 230, holding for 12 minutes, t2> 10, where vi <v2 <V3.
    [3]
    A method for identifying characteristic volatile compounds in meat or meat products according to claim 1, characterized in that a headspace solid phase micro-extraction process is used as the method for extracting volatile compounds in meat or meat products, the extraction process comprising: weighing meat or meat product, adding a saturated sodium chloride solution to the meat or meat product in a 1 ml 1 g ratio, adding a standard organic compound, stirring evenly, preheating for 8-15 minutes at 40 - 60 ° C, and adsorbing by means of a CAR / PDMS extraction needle at 40 - 60 ° C for 40 - 60 minutes.
    [4]
    A method for identifying characteristic volatile compounds in meat or meat products according to claim 2, characterized in that the process of qualitatively detecting specific components of volatile compounds by gas chromatography-olfactometry-mass spectrometry comprises: recovery by means of of a mass spectrometric library, calculating the retention index, analyzing by olfactometry, and performing a standard qualitative analysis to obtain specific components of volatile compounds.
    [5]
    Method for identifying characteristic volatile compounds in meat or meat products according to claim 4, characterized in that the process of quantitative detection of the concentration of each component in gas chromatography-olfactometry-mass spectrometry comprises: preparing a plurality of odorless meat or meat product matrices, detecting each component in volatile compounds by gas chromatography olfactometry mass spectrometry, taking a standard sample to prepare a mixed standard solution 3 of different concentration, adding the mixed standard solution 3 of different concentration to the multitude of odorless meat or meat product matrices, extracting volatile compounds from any of the meat or meat product matrices containing the mixed standard solution 3 by means of the headspace solid phase micro-extraction process, detecting the pielc surface of characteristic e ion fragments of each component by gas chromatography-olfactometry-mass spectrometry, drawing up a standard curve comparison between the peak area of characteristic ion fragments and the concentration of each component in volatile compounds, and determining the concentration of each component in volatile compounds of meat or meat products according to the peak area of characteristic ion fragments of each component in volatile compounds of meat or meat products detected by the gas chromatography-olfactometry-mass spectrometry.
    [6]
    A method for identifying characteristic volatile compounds in meat or meat products according to claim 1 or 5, characterized in that a method for preparing odorless meat or meat product matrices comprises: weighing meat or meat product, mixing the meat or meat product, diethyl ether and n-pentane in a ratio of 1 g: 2 ml: 1 ml, shaking the resulting mixture in a shaker, filtering, removing organic solution, repeating the operation several times until the meat or meat product is odorless, freezing and drying the odorless meat or meat product, and adding purified water thereto, the amount of purified water added being consistent with the water content of the meat or meat product. 19
    [7]
    Method for identifying characteristic volatile compounds in meat or meat products according to claim 1, characterized in that the sensory analysis triangle test is used as a method for comparing the taste of the recombination model 1 with the recombination model 2.
    [8]
    Method for identifying characteristic volatile compounds in meat or meat products according to claim 1, characterized in that the preset value a is 90% and the preset value b is 1.
    [9]
    Method for identifying characteristic volatile compounds in meat or meat products according to claim 2, characterized in that the capillary column of the gas chromatography olfactometry mass spectrometry is DB-Wax and the heating process comprises: maintaining at the initial column temperature of 40 ° C for 3 minutes, heating to 70 ° C at a speed of 2 ° C / min, heating to 130 ° C at a speed of 3 ° C / min, heating to 230 ° C at a speed of 10 ° C / min, and holding for 10 minutes.
    [10]
    Method for identifying characteristic volatile compounds in meat or meat products according to claim 3, characterized in that the process for extracting volatile compounds from meat or meat products comprises: weighing meat or meat product, adding a saturated sodium chloride solution to the meat or meat product in a ratio of 1 ml: 1 g, adding a standard sample of 2-methyl-3-heptanone, placing a magnetic rotor to perform magnetic stirring, uniform stirring, preheating for 10 min at 55 ° C, and adsorbing through a 75 µm CAR / PDMS extraction needle at 55 ° C for 45 minutes.
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    同族专利:
    公开号 | 公开日
    CN109696501A|2019-04-30|
    NL2022959B1|2020-11-26|
    CN109696501B|2021-12-07|
    引用文献:
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    CN102520100A|2011-12-13|2012-06-27|中国农业科学院农产品加工研究所|Auxiliary identification method of geographical origin of beef|
    US9188568B2|2012-02-14|2015-11-17|The Regents Of The University Of California|Gas chromatography recomposition-olfactometry for characterization of aroma mixtures|
    CN105572286A|2016-01-22|2016-05-11|浙江大学|Determination method for turtle fishy smell matter|
    CN105823836A|2016-03-11|2016-08-03|中国农业科学院农产品加工研究所|Sauce braised meat product flavor active substance profile analysis method|
    CN108008055A|2017-11-29|2018-05-08|北京工商大学|A kind of method for quick identification of diced mutton flavouring essence quality|CN110487947A|2019-09-19|2019-11-22|中国农业科学院农产品加工研究所|Identify the method for hiding pig and its meat products based on chemometrics application|
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    申请号 | 申请日 | 专利标题
    CN201910100485.4A|CN109696501B|2019-01-31|2019-01-31|Method for identifying characteristic volatile flavor substances of meat or meat products|
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