CN103105440A - Method for identifying volatile flavor substance in bolete - Google Patents
Method for identifying volatile flavor substance in bolete Download PDFInfo
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- CN103105440A CN103105440A CN2012104370028A CN201210437002A CN103105440A CN 103105440 A CN103105440 A CN 103105440A CN 2012104370028 A CN2012104370028 A CN 2012104370028A CN 201210437002 A CN201210437002 A CN 201210437002A CN 103105440 A CN103105440 A CN 103105440A
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Abstract
The invention relates to a method for measuring a volatile flavor substance in bolete. The method comprises the following steps of: (1) extracting volatile components in the bolete by adopting a headspace solid-phase micro-extraction (HS-SPME) method; (2) separating and identifying the extracted volatile components by combining a Kovats keeping index (KI) by utilizing a gas chromatography-mass spectrography technology; and (3) identifying the volatile flavor substance in bolete by utilizing a gas chromatography-olfaction (GC-O) measurement method. According to the method, the volatile flavor substance in bolete can be simply and rapidly analyzed, an organic solvent is not required by adopting the HS-SPME method, the phenomenon that the sample volatilizes in the heating process and other substances are generated is avoided, and the volatile components are effectively collected; and moreover, the volatile compound to be tested is accurately identified by combining three methods including mass spectrogram analysis, retention index and olfaction identification, and the reliability of the result is improved.
Description
Technical field
The invention belongs to technical field of food science, belong to the edible fungus flavor analysis technical field, be specifically related to headspace solid-phase microextraction-gas chromatography-mass spectrography technology and gas chromatography-olfactometry technology.
Background technology
Bolete is the meat macro fungi, it is the important monoid of the medium-and-large-sized basidiomycetes of fungus circle, its typical external appearance characteristic is: have cap and stem, meat, with agaric (mushroom) appearance similar, but the fructification layer below cap is intensive tube but not sheet lamella.The bolete fructification is glued soft succulence, and is fragrant sliding good to eat, is rich in protein vitamin polysaccharose substance amino acid and several kinds of mineral elements, and its extract has the functions such as the anticancer radioresistance of the immunity of enhancing.Except nutrition and medicinal, edible bolete local flavor also noticeable, its peculiar local flavor is different from fragrant plant and normal food.In recent years, along with the transformation of growth in the living standard and consumption idea, people increase day by day to the pursuit of flavour of food products when pursue taking in food nutrition.The wild edible bolete has been satisfied the dual requirements of consumer for nutrition and local flavor, more and more comes into one's own in the consumption market, China and foreign countries.In Yunnan and some other provinces, a lot of restaurants begin to cook soup with the wild edible bolete, and its delicious flavour is liked by the consumer deeply.Simultaneously, bolete is the European market rare food of welcoming extremely, and it is particularly praised highly in Italy, France, Switzerland, Germany etc., is that special product product in the situation of selling well of European and American countries are found a good sale in by China.Therefore, for the research of wild edible bolete flavor components, be flavor mechanism and for Development of New Generation flavouring based theoretical, have far-reaching realistic meaning for illustrating it.
At present, more about the research of bolete nutritional labeling, and less for its volatile ingredient research.Headspace solid-phase microextraction (headspace-solid phase micro-extraction, HS-SPME) is a kind of technology for the food flavor substances analyzing and testing that the nineties in 20th century, new development was got up.The characteristics of this method maximum are that the processes such as sampling, extraction, enrichment, sample introduction are completed at same device, have reduced the loaded down with trivial details of experiment.Compare with other separation methods, the method selectivity is good, does not need solvent, and required amount of samples is few, and simple to operate, quick, expense is low, and can with gas chromatography or the direct coupling of liquid chromatography.At present existing Chinese scholars is used the volatile matter that solid-phase microextraction technology (SPME-GC-MS) has been analyzed the edible fungis such as Asparagus, straw mushroom, mushroom.
Above method has just carried out separating evaluation to the volatile matter of food, but can not determine which kind of composition has contribution to flavour of food products, this is because in a large amount of volatile compounds, the local flavor that often only has sub-fraction composition influence food, and some taste compound threshold value is very low, content is very little in food, the simple GC-MS technology of using often can not detect these trace flavor substances, and gas chromatography-olfactometry (GC-O) makes the research of flavour of food products that very large breakthrough arranged.This experiment is take cepe as raw material, by the volatile ingredient in HS-SPME technology extraction sample, and with GC-MS and GC-O and Kovats retention index (Kovats retention indices, KI) three kinds of methods combine, volatile ingredient in sample is carried out qualitative and quantitative analysis, identify simultaneously the flavor components in sample, for the exploitation of bolete flavouring provides certain theoretical foundation.
By retrieval, not yet find publication document related with the present patent application.
Summary of the invention
The assay method that the purpose of this invention is to provide a kind of bolete volatile flavor substance.
The present invention realizes that the technical scheme of purpose is:
A kind of method of identifying the bolete volatile flavor substance, concrete steps are:
(1) the bolete dry product is pulverized, crossed 40 mesh sieves;
(2) adopt the headspace solid-phase microextraction method to carry out sorption extraction to volatile ingredient;
(3) utilize gas chromatography-gas chromatography mass spectrometry technology that volatile ingredient is identified;
(4) utilize the osmesthesia method to further determining volatile ingredient, determine that by odour intensity each material is to the size of bolete local flavor contribution simultaneously.
And, adopting 65 μ m PDMS/DVB extracting head in described step (2), optimum extraction time is 30min, best extraction temperature is 45 ℃.
And, in described step (3), GC conditions is: the chromatographic column model is VF-5ms (30m * 0.25mm * 0.25 μ m), and carrier gas is high-purity helium (99.999%), and flow velocity is 1ml/min, injector temperature is 250 ℃, during sample introduction with the shunting mode sample introduction.Adopt the two-part temperature programme: initial temperature is 40 ℃, keeps 3min, then is warming up to 150 ℃ with 4.0 ℃ of min, and keeps 1min, then is warming up to 250 ℃ with 8 ℃/min, keeps 6min.The mass spectrum condition is: ionization source is EI, and the ion trap temperature is 220 ℃, and GC-MS transmission line temperature is 280 ℃, and the EI electron energy is 70eV, solvent delay time 1.5min.Scan mode is full scan (f μ μ), and scope is 43-500m/z.
And the osmesthesia method concrete steps in described step (4) are: the split ratio of mass spectrum and osphresiometer is set to 1:1.3 experienced sensory evaluation persons of this experimental selection carry out olfactory analysis, record flavor characteristic and intensity.Have at least two sensory evaluation persons can obtain identical sense organ and describe at the same news time place of smelling in experimentation, net result charged in this record, the intensity of smell is marked with the asterisk number.
The volatile flavor component of the method that the present invention sets up in can the analysis bolete of Simple fast, adopt the HS-SPME method not need organic solvent, simple to operate, avoided sample in heating process volatilization and produce other material, can effectively collect volatile ingredient; Utilize mass spectrogram analysis, retention index and three kinds of methods of osmesthesia in conjunction with precise Identification volatile compound to be measured, improved the confidence level of result; Analyze simultaneously the odour intensity of volatile compound by olfactometry, determine the impact on the whole local flavor of bolete.
Description of drawings
Fig. 1 is the total ion chromatogram of bolete volatile ingredient.
Embodiment
The below is described in detail embodiments of the invention, need to prove, the present embodiment is narrative, is not determinate, can not limit protection scope of the present invention with this.
A kind of detection method of bolete volatile flavor substance, step is:
(1) the bolete dry product is pulverized, crossed 40 mesh sieves;
(2) take sample powder 2.0g in 15ml headspace sample bottle, silicone rubber pad sealing with teflon lined, after being placed in 45 ℃ of water-bath balance 30min, will be through the existing solid phase micro-extracting head of overaging place the rubber gasket by bottle cap be inserted in sample bottle approximately 1cm place, release fiber head, extract 30min in 45 ℃ of water-baths, then draw back fiber head, insert rapidly the injection port of GC-MS combined instrument take out extracting head from sample bottle after, resolve 15min under 250 ℃, start simultaneously the instrument image data;
(3) GC-MS analysis condition
Chromatographic condition: the chromatographic column model is VF-5ms (30m * 0.25mm * 0.25 μ m), and carrier gas is high-purity helium (99.999%), and flow velocity is 1ml/min, and injector temperature is 250 ℃, during sample introduction with the shunting mode sample introduction.Adopt the two-part temperature programme: initial temperature is 40 ℃, keeps 3min, then is warming up to 150 ℃ with 4.0 ℃ of min, and keeps 1min, then is warming up to 250 ℃ with 8 ℃/min, keeps 6min.
The mass spectrum condition: ionization source is EI, and the ion trap temperature is 220 ℃, and GC-MS transmission line temperature is 280 ℃, and the EI electron energy is 70eV, solvent delay time 1.5min.Scan mode is full scan (f μ μ), and scope is 43-500m/z.
(4) qualitative analysis
Data Processing in Experiment is completed by the Xaclbiur software systems, the fine computer search of unknown compound is complementary with NSIT05 spectrum storehouse (107k compounds) simultaneously, only works as positive and negative matching degree and is all just reported greater than the qualification result of 800 (maximal value is 1000).Adopt identical heating schedule, with C
6-C
20N-alkane as standard, with the retention index of the compound in the test of its retention time calculation sample, then by consulting pertinent literature, compare with the retention index (RI) of compound in document, jointly qualitative with mass spectrometric data library searching result.
Compound retention index RI computing formula:
RI
Sample=RI
Before+ (Rt
Sample-Rt
Before) * 100/ (Rt
After-Rt
Before)
RI in formula
Sample---the RI at sample chromatogram peak;
RI
Before---the RI of front, sample chromatogram peak alkane standard specimen;
Rt
Sample---the Rt at sample chromatogram peak;
Rt
BeforeThe Rt of-front alkane standard specimen;
Rt
After---the Rt of back alkane standard specimen;
The retention time of Rt---chromatographic peak.
(5) quantitative test
By the Xaclbiur workstation data processing system, carry out quantitative test by areas of peak normalization method, thereby draw the relative percentage composition of each chemical composition in the bolete material.
(6) GC-O analyzes
The split ratio of mass spectrum and osphresiometer is set to 1:1.3 experienced sensory evaluation persons of this experimental selection carry out olfactory analysis, record flavor characteristic and intensity.Have at least two sensory evaluation persons can obtain identical sense organ and describe at the same news time place of smelling in experimentation, net result charged in this record, the intensity of smell is marked with the asterisk number.
Table 1 is analysis and the qualification result of characteristic volatile compound in bolete.
The analysis of characteristic volatile compound and qualification result in table 1 bolete
Annotate: the MS-compound is through Mass Spectrometric Identification; The RI of RI-actual measurement RI and standard items coincide; RIL-sample RI and bibliographical information value are coincide; The Aroma-compound is identified through smelling to hear
By table 1 as can be known, use HS-SPME method is extracted the volatile ingredient of Yunnan Wild bolete, by GC-MS, its volatile ingredient is analyzed again, and identify 53 kinds of compounds in conjunction with retention index, 12 kinds of pyrazine compounds are wherein arranged, accounting for 58.87% of general volatile composition, is the main volatile composition of bolete.The compound that in the bolete volatile ingredient, content is higher has 2,6-dimethyl pyrazine (30.09%), 3-ethyl-2,5-dimethyl pyrazine (13.32%), 2 thiophene carboxaldehyde (10.50%), 2-ethyl-3-methylpyrazine (5.35%), 2-ethyl-6-methylpyrazine (4.06%), third valerolactone (3.34%), hexanal (2.54%), 2-n-pentyl furans (2.30%) etc.
Identify the characteristic volatile matter of Yunnan Wild bolete by the GC-O method, obtain altogether 32 kinds of Flavoring Components, wherein have 3 kinds of materials not detect by GC-MS.by the odour intensity of bolete characteristic volatile compound is carried out record, odour intensity is larger mainly contains hexanal (herbaceous taste), methylpyrazine (nutty flavor), 3-methylthiopropionaldehyde (burnt odor), 2,6-dimethyl pyrazine (barbecue is fragrant), 1-OCOL (mushroom taste), 2-amyl furan (beans are fragrant), 2-ethyl-6-methylpyrazine (roasting fragrant), 3-octene-2-ketone (mushroom taste), the compounds such as phenylacetaldehyde (fragrance of a flower), they are very large to the whole local flavor contribution of bolete, it is main characteristic volatile matter.
Claims (5)
1. the authentication method of a bolete volatility flavor substance, it is characterized in that: adopt the volatile ingredient in headspace solid-phase microextraction technology extraction bolete, then by gas chromatograph-mass spectrometer (GCMS), composition to be measured is carried out quantitatively and qualitative analysis, in conjunction with the volatile compound of waving in retention index evaluation bolete, utilize at last gas chromatography-olfactometry further to determine the volatility constituent, describe with odour intensity by sense organ simultaneously and determine that each compound is to the size of the whole local flavor contribution of bolete.
2. the authentication method of bolete volatile flavor substance according to claim 1, it is characterized in that: in described headspace solid-phase microextraction step, extraction time is 20-40 minute, be defined as 30 minutes, extraction temperature is 30 ℃-60 ℃, preferred 45 ℃, uses 65 μ m PDMS/DVB extracting head.Get the 1g sample and be placed in 15ml head space bottle, after 45 ℃ of water-bath balance 30min, will be through the solid phase micro-extracting head of burin-in process the rubber gasket by bottle cap be inserted in sample bottle approximately 1cm place, the release fiber head extracts 30min in 45 ℃ of water-baths.
3. the authentication method of bolete volatile flavor substance according to claim 1, it is characterized in that: in the gas chromatography-mass spectrum detecting step, after extraction is completed, extracting head is inserted into the injection port of gas chromatography, resolves 5min under 250 ℃, start simultaneously the instrument image data.The chromatographic column model is VF-5ms (30m * 0.25mm * 0.25 μ m), and carrier gas is high-purity helium (99.999%), and flow velocity is 1ml/min, and injector temperature is 250 ℃, during sample introduction with the shunting mode sample introduction.Adopt the two-part temperature programme: initial temperature is 40 ℃, keeps 3min, then is warming up to 150 ℃ with 4.0 ℃ of min, and keeps 1min, then is warming up to 250 ℃ with 8 ℃/min, keeps 6min.The mass spectrum condition: ionization source is EI, and the ion trap temperature is 220 ℃, and GC-MS transmission line temperature is 280 ℃, and the EI electron energy is 70eV, solvent delay time 1.5min.Scan mode is full scan (f μ μ), and scope is 43-500m/z.
4. the authentication method of bolete volatile flavor substance according to claim 1, it is characterized in that: in characteristic flavor substance authentication step, the split ratio of mass spectrum and osphresiometer is set to 1:1.3 experienced sensory evaluation persons of this experimental selection carry out olfactory analysis, record flavor characteristic and intensity.Have two sensory evaluation persons at least obtaining identical sense organ and describe at the same news time place of smelling in testing toothed oak, net result charged in this record, the intensity of smell is marked with the asterisk number.
5. the authentication method of ox bacterium volatile flavor substance according to claim 1, it is characterized in that: in the qualitative analysis step of volatile ingredient, utilize mass spectrogram analysis, retention index and three kinds of methods of osmesthesia in conjunction with precise Identification volatile compound to be measured.
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| CN104360034A (en) * | 2014-10-22 | 2015-02-18 | 无限极（中国）有限公司 | Method for analyzing and discriminating odorous substances in drinking water |
| CN106645495A (en) * | 2016-12-29 | 2017-05-10 | 中粮集团有限公司 | Detection method for volatile components of sugar |
| CN107179375A (en) * | 2017-07-06 | 2017-09-19 | 浙江大学 | A kind of method of volatile flavor substance in ultrasonic method auxiliary measuring brown rice |
| WO2019114052A1 (en) * | 2017-11-12 | 2019-06-20 | 华南农业大学 | Artificial intelligence-based food flavor sensory evaluation system and establishment method therefor |
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| CN112198256A (en) * | 2020-09-30 | 2021-01-08 | 广东省农业科学院蚕业与农产品加工研究所 | Method for rapidly detecting chestnut smell and application thereof |
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Non-Patent Citations (12)
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| CN104360034A (en) * | 2014-10-22 | 2015-02-18 | 无限极（中国）有限公司 | Method for analyzing and discriminating odorous substances in drinking water |
| CN104360034B (en) * | 2014-10-22 | 2017-03-15 | 无限极（中国）有限公司 | A kind of analysis and distinguishing method of abnormal flavour thing in drinking water |
| CN106645495A (en) * | 2016-12-29 | 2017-05-10 | 中粮集团有限公司 | Detection method for volatile components of sugar |
| CN107179375B (en) * | 2017-07-06 | 2020-02-21 | 浙江大学 | Method for measuring volatile flavor substances in brown rice with assistance of ultrasonic method |
| CN107179375A (en) * | 2017-07-06 | 2017-09-19 | 浙江大学 | A kind of method of volatile flavor substance in ultrasonic method auxiliary measuring brown rice |
| WO2019114052A1 (en) * | 2017-11-12 | 2019-06-20 | 华南农业大学 | Artificial intelligence-based food flavor sensory evaluation system and establishment method therefor |
| CN110531005A (en) * | 2019-10-14 | 2019-12-03 | 贵州省分析测试研究院 | A method of detection mountainous region rose aroma ingredient |
| CN112198256A (en) * | 2020-09-30 | 2021-01-08 | 广东省农业科学院蚕业与农产品加工研究所 | Method for rapidly detecting chestnut smell and application thereof |
| CN113341022A (en) * | 2021-06-29 | 2021-09-03 | 湖北中烟工业有限责任公司 | Method for analyzing peculiar smell components in packaging material |
| CN113740475A (en) * | 2021-09-02 | 2021-12-03 | 天津春发生物科技集团有限公司 | Construction method of green pepper GC-MC fingerprint |
| CN115047091A (en) * | 2022-04-06 | 2022-09-13 | 中华全国供销合作总社济南果品研究所 | Analysis method for aroma components in dried red date slices |
| CN115290804A (en) * | 2022-08-18 | 2022-11-04 | 天津春发生物科技集团有限公司 | Fingerprint spectrum of allspice extract for food and construction method thereof |
| CN115406999A (en) * | 2022-10-11 | 2022-11-29 | 湖北省农业科学院经济作物研究所 | Method for detecting and analyzing phellinus igniarius flavor substances |
| CN115508486A (en) * | 2022-10-19 | 2022-12-23 | 天津春发生物科技集团有限公司 | Method for determining flavor substances in chicken soup based on SAFE-GC-MS technology and application thereof |
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Application publication date: 20130515 |