CN102279230A - Method for establishing volatile ingredient fingerprint map of agricultural product and processed product of agricultural product - Google Patents
Method for establishing volatile ingredient fingerprint map of agricultural product and processed product of agricultural product Download PDFInfo
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- CN102279230A CN102279230A CN2011101225009A CN201110122500A CN102279230A CN 102279230 A CN102279230 A CN 102279230A CN 2011101225009 A CN2011101225009 A CN 2011101225009A CN 201110122500 A CN201110122500 A CN 201110122500A CN 102279230 A CN102279230 A CN 102279230A
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Abstract
The invention belongs to the technical field of food chemical pattern identification, in particular relates to a method for establishing a volatile ingredient fingerprint map of an agricultural product and a processed product of the agricultural product. The main expression form of the current fingerprint map on food chemical pattern identification is a map formed by colour spectrum outflow curves of chemical ingredients in a geographic indication product, people can not directly obtain information related to product quality, and the fingerprint map can not be easily and visually understood, thus application and popularization of the fingerprint map are restricted, especially when an analysis system is complex. In the invention, volatile ingredients which can express aesthetic quality and style characteristic of the agricultural product and the processed product of the agricultural product are used for expressing fingerprint characteristic of an analyzed sample, and a chemical pattern characteristic fingerprint map which can visually express an analysis object is established to identify characteristic and flavour of an object. The volatile ingredient fingerprint map established by the method provided by the invention can be taken as an objective chemical information bar code of the agricultural product, and symbolic effect for expressing specificality of the agricultural product is obvious.
Description
Technical field
The invention belongs to the Food Chemistry mode identification technology, be specifically related to the method for building up of a kind of agricultural product and converted products volatile ingredients fingerprint thereof.
Background technology
The quality of agricultural product and converted products thereof and feature thereof and style depend mainly on the natural cause and the human factors such as cultivation management measure, processing technology such as weather, geology, soil and overdone cultivar in original producton location.Chemical constitution and flavor characteristic complicated in agricultural product and the converted products thereof are closely connected, and they have constituted the objective quality of product jointly.The external history in existing more than 100 year of geographical sign product protection system of implementing; the product of implementing protection system the earliest is a grape wine; the country of grape wine industry prosperity in the world; all formulate and the rules of having implemented the name protection of relevant grape wine geographical sign and original producton location, promoted the sound development of grape and grape wine industry forcefully.China introduced this system in 1999, and had issued " geographical sign product protection regulation " with the form of former National Quality ﹠ Technology Inspection Bureau the 6th command.But original producton location name at present and protection system thereof are at the early-stage, comprehensive legislation in the industry are not carried out in the protection of geographical famous special product as yet, and relevant laws and regulations are perfect not enough, and be not strong to the dynamics of the geographical sign product protection of agricultural product and converted products thereof.Cause China's product quality of class geographical sign product on market very different, be no lack of the phenomenon that ichthyosauru mixes pearl.The Chemical Pattern Recognition enforcement in industry of China's geographical sign product starts from National Drug Administration's promulgation in 2000 " technical requirement of traditional Chinese medicine finger-print research " the earliest, and the fingerprint pattern technology research about agricultural product and converted products thereof subsequently also becomes focus.But the main forms of these finger-prints is formed spectrograms of chromatogram elution curve of chemical constitution in the geographical sign product, people can not directly obtain the relevant information about product quality, be difficult for intuitivism apprehension, particularly when analysis system is very complicated, has limited this class Application of Fingerprint and promoted.
Summary of the invention
The purpose of this invention is to provide and a kind ofly can analyze and utilize the agricultural product of chemical composition of the whole reflection of the cognizable gray-scale map of vision various kinds product and the method for building up of converted products volatile ingredients fingerprint thereof the volatile ingredient of agricultural product and converted products thereof, with this novel chemical information bar codes technique, the chemistry model difference of expression analysis object intuitively.
The technical solution adopted in the present invention is:
The method for building up of a kind of agricultural product and converted products volatile ingredients fingerprint thereof is characterized in that:
Realize by following steps:
Step 1: analyze geographical sign product producing region in plan and carry out the liquid phase sample collection, record product kind, time, processing technology, producer's information;
Step 2: adopt solid phase micro-extraction method, liquid phase sample is carried out the extracting and enriching of volatile ingredient;
Step 3: the volatile ingredient to enrichment in the step 2 carries out gas chromatography-mass spectrometry analysis, promptly volatile ingredient is carried out qualitative and quantitative analysis, obtains the quantized data [X of volatile ingredient
Ij], wherein X represents the concentration of volatile ingredient, and i represents sample number into spectrum, and j represents the volatile ingredient sequence number, and the concentration of volatile ingredient is arranged according to chromatographic retention;
Step 4: the quantized data [X of the volatile ingredient that step 3 is obtained
Ij] carry out standardization, at first, to data matrix [X
Ij] carrying out the translation processing, matrix [X fetches data
Ij] data minimum value X in each column vector
j Min, make following translation transformation and obtain [Y
Ij];
Y
ij=?X
ij-X
j min
Then, the translation data are carried out normalized, matrix [Y fetches data
Ij] in data maximal value Y
Max, make following compressed transform and obtain [Z
Ij], it is [0, a 1] hypercube;
Z
ij=?Y
ij/Y
max
Step 5: with data matrix [Z
Ij] in numerical value and linear gray-scale map in the different gray scale depths between corresponding one by one, carry out space projection, obtain the finger-print of volatile ingredient, the coordinate position of the X axle in the collection of illustrative plates is represented the chromatographic retention of volatile ingredient in the sample, and the Y axle of gray-scale map is complementary scalar.
In the described step 1, the liquid phase sample collection is meant that working as product is that desirable succulent fruits is real-time, and squeezing the juice obtains liquid phase sample; When if product is solid-state inadvisable juice agricultural product, pulverizing the back, to adopt massfraction be that 99.8% alcohol solution dipping obtains liquid phase sample; When if product is the beverage series products, directly as liquid phase sample.
The concrete steps of the solid phase micro-extraction method in the described step 2 are: add liquid phase sample 10 mL, sodium chloride and internal standard compound matter 3-octanol in the head space bottle of magnetic stir bar is housed, make that the mass volume concentrations of sodium chloride is 2.0 g/L, the mass volume concentrations of internal standard compound matter 3-octanol is 0.4mg/L; Balance is 10 minutes under 40 ℃ of conditions, inserts 100 μ m polydimethylsiloxone extracting fibers, adsorbs 30～40 minutes under 40 ℃ of conditions again.
Quantized data [the X of volatile ingredient in the described step 3
Ij] be the sxemiquantitative data of volatile ingredient with respect to the 3-octanol, these sxemiquantitative data equal the mass volume concentrations that volatile ingredient characteristic ion peak area and the ratio of 3-octanol peak area multiply by internal standard compound matter 3-octanol; With the place of production or with the kind sample, get 10 batches of sample analysis, calculate average result.
The present invention has the following advantages:
The present invention adopts the fingerprint characteristic of the volatile ingredient expression analysis sample that can represent agricultural product and processed goods aesthetic quality and style characteristic thereof, sample pretreatment is simple, and sample is not had extra process, does not damage original flavor quality, the preparation method of chromatographic data is fast and simple, reliable science; The sign of finger-print adopts the volatile constituent of the whole reflection of the cognizable gray-scale map of vision sample, the chemistry model feature of expression analysis object directly perceived is set up finger-print, this method can be used as objectively chemical information bar code of product itself, and the significant effect of expressing the product uniqueness is very obvious.
Description of drawings
Fig. 1 is a process flow diagram of the present invention.
Fig. 2 is the finger-print of producing region, Changli, Hebei Cabernet Sauvignon claret in 2005.
Fig. 3 is the finger-print of Manas producing region, Xinjiang Cabernet Sauvignon claret in 2005.
Fig. 4 is the finger-print of Muller producing region, Yunnan Cabernet Sauvignon claret in 2005.
Fig. 5 is the finger-print of producing region, the foot of a hill or mountain, Shandong, Helan Cabernet Sauvignon claret in 2005.
Fig. 6 is the finger-print of producing region, Shachen City Cabernet Sauvignon claret in 2005.
Among the figure, the coordinate position of X axle is represented the chromatographic retention of volatile ingredient, and Y-axis is complementary scalar.
Embodiment
The present invention will be described in detail below in conjunction with embodiment.
A kind of agricultural product involved in the present invention and the method for building up of converted products volatile ingredients fingerprint thereof, realize by following steps:
Step 1: analyze geographical sign product producing region in plan and carry out the liquid phase sample collection, record product kind, time, processing technology, producer's information.The liquid phase sample collection is meant that working as product is that desirable succulent fruits is real-time, and squeezing the juice obtains liquid phase sample; When if product is solid-state inadvisable juice agricultural product, pulverizing the back, to adopt massfraction be that 99.8% alcohol solution dipping obtains liquid phase sample; When if product is the beverage series products, directly as liquid phase sample.
Step 2: adopt solid phase micro-extraction method, liquid phase sample is carried out the extracting and enriching of volatile ingredient.The concrete steps of solid phase micro-extraction method are: add liquid phase sample 10 mL, sodium chloride and internal standard compound matter 3-octanol in the head space bottle of magnetic stir bar is housed, make that the mass volume concentrations of sodium chloride is 2.0 g/L, the mass volume concentrations of internal standard compound matter 3-octanol is 0.4mg/L; Balance is 10 minutes under 40 ℃ of conditions, inserts 100 μ m polydimethylsiloxone extracting fibers, adsorbs 30～40 minutes under 40 ℃ of conditions again.
Step 3: the volatile ingredient to enrichment in the step 2 carries out gas chromatography-mass spectrometry analysis.Analysis condition is: DB-Wax capillary column, i.e. 30m * 0.32mm i.d., capillary coating thickness 0.25 μ m; Carrier gas: He; Flow velocity: 1ml/min; Heating schedule: 40 ℃ kept 3 minutes, rose to 160 ℃ with 4 ℃/min speed then, rose to 230 ℃ with 7 ℃/min speed again, kept 8 minutes at 230 ℃; Connecting link temperature: 230 ℃; Injector temperature: 250 ℃.The mass spectrum condition is: EI+ ionization source, ion source temperature are 230 ℃, and electron energy is 70eV, and the filament flow is 0.20 mA, and detector voltage is 350V, and sweep limit is 33～450 amu, 1 time/s of sweep speed.Above condition also can be optimized debugging at different testing samples.This step is that volatile ingredient is carried out qualitative and quantitative analysis, in the qualitative analysis, the Mass Spectrometer Method peak adopt the gas chromatograph-mass spectrometer (GCMS) device at random with compound library searching method qualitative, qualitative foundation is a matching degree greater than 800 material; Quantitative test can obtain the quantized data [X of volatile ingredient
Ij], the quantized data [X of volatile ingredient
Ij] be the sxemiquantitative data of volatile ingredient with respect to the 3-octanol, these sxemiquantitative data equal the mass volume concentrations that volatile ingredient characteristic ion peak area and the ratio of 3-octanol peak area multiply by internal standard compound matter 3-octanol; With the place of production or with the kind sample, get 10 batches of sample analysis, calculate average result.Wherein X represents the concentration of volatile ingredient, and i represents sample number into spectrum, and j represents the volatile ingredient sequence number, and the concentration of volatile ingredient is arranged according to chromatographic retention.
Step 4: the quantized data [X of the volatile ingredient that step 3 is obtained
Ij] carry out standardization, at first, to data matrix [X
Ij] carrying out the translation processing, matrix [X fetches data
Ij] data minimum value X in each column vector
j Min, make following translation transformation and obtain [Y
Ij];
Y
ij=?X
ij-X
j min
Then, the translation data are carried out normalized, matrix [Y fetches data
Ij] in data maximal value Y
Max, make following compressed transform and obtain [Z
Ij], it is [0, a 1] hypercube.
Z
ij=?Y
ij/Y
max
Step 5: with data matrix [Z
Ij] in numerical value and linear gray-scale map in the different gray scale depths between corresponding one by one, carry out space projection, obtain the finger-print of volatile ingredient, the coordinate position of the X axle in the collection of illustrative plates is represented the chromatographic retention of volatile ingredient in the sample, the Y axle of gray-scale map is complementary scalar, by above step, the one-dimensional data vector is converted to 2 d plane picture, and the grey graph region of a certain volatile ingredient begins to end to the retention time of next volatile ingredient from its retention time.
Fig. 2-6 is the finger-print of Changli, China Hebei of adopting the present invention to set up, Xinjiang Manas, Yunnan Muller, 5 producing regions in the foot of a hill or mountain, Shandong, Helan and Shachen City, Hebei Cabernet Sauvignon claret in 2005 product, can present the difference of different producing regions Cabernet Sauvignon claret product intuitively.
Claims (4)
1. the method for building up of agricultural product and converted products volatile ingredients fingerprint thereof is characterized in that:
Realize by following steps:
Step 1: analyze geographical sign product producing region in plan and carry out the liquid phase sample collection, record product kind, time, processing technology, producer's information;
Step 2: adopt solid phase micro-extraction method, liquid phase sample is carried out the extracting and enriching of volatile ingredient;
Step 3: the volatile ingredient to enrichment in the step 2 carries out gas chromatography-mass spectrometry analysis, promptly volatile ingredient is carried out qualitative and quantitative analysis, obtains the quantized data [X of volatile ingredient
Ij], wherein X represents the concentration of volatile ingredient, and i represents sample number into spectrum, and j represents the volatile ingredient sequence number, and the concentration of volatile ingredient is arranged according to chromatographic retention;
Step 4: the quantized data [X of the volatile ingredient that step 3 is obtained
Ij] carry out standardization, at first, to data matrix [X
Ij] carrying out the translation processing, matrix [X fetches data
Ij] data minimum value X in each column vector
j Min, make following translation transformation and obtain [Y
Ij];
Y
ij=?X
ij-X
j min
Then, the translation data are carried out normalized, matrix [Y fetches data
Ij] in data maximal value Y
Max, make following compressed transform and obtain [Z
Ij], it is [0, a 1] hypercube;
Z
ij=?Y
ij/Y
max
Step 5: with data matrix [Z
Ij] in numerical value and linear gray-scale map in the different gray scale depths between corresponding one by one, carry out space projection, obtain the finger-print of volatile ingredient, the coordinate position of the X axle in the collection of illustrative plates is represented the chromatographic retention of volatile ingredient in the sample, and the Y axle of gray-scale map is complementary scalar.
2. the method for building up of agricultural product according to claim 1 and converted products volatile ingredients fingerprint thereof is characterized in that:
In the described step 1, the liquid phase sample collection is meant that working as product is that desirable succulent fruits is real-time, and squeezing the juice obtains liquid phase sample; When if product is solid-state inadvisable juice agricultural product, pulverizing the back, to adopt massfraction be that 99.8% alcohol solution dipping obtains liquid phase sample; When if product is the beverage series products, directly as liquid phase sample.
3. the method for building up of agricultural product according to claim 1 and converted products volatile ingredients fingerprint thereof is characterized in that:
The concrete steps of the solid phase micro-extraction method in the described step 2 are: add liquid phase sample 10 mL, sodium chloride and internal standard compound matter 3-octanol in the head space bottle of magnetic stir bar is housed, make that the mass volume concentrations of sodium chloride is 2.0 g/L, the mass volume concentrations of internal standard compound matter 3-octanol is 0.4mg/L; Balance is 10 minutes under 40 ℃ of conditions, inserts 100 μ m polydimethylsiloxone extracting fibers, adsorbs 30～40 minutes under 40 ℃ of conditions again.
4. the method for building up of agricultural product according to claim 1 and converted products volatile ingredients fingerprint thereof is characterized in that:
Quantized data [the X of volatile ingredient in the described step 3
Ij] be the sxemiquantitative data of volatile ingredient with respect to the 3-octanol, these sxemiquantitative data equal the mass volume concentrations that volatile ingredient characteristic ion peak area and the ratio of 3-octanol peak area multiply by internal standard compound matter 3-octanol; With the place of production or with the kind sample, get 10 batches of sample analysis, calculate average result.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102621193A (en) * | 2012-03-25 | 2012-08-01 | 上海市农业科学院 | Finger-print chromatogram for flavor composition of edible mushroom |
| CN103217487A (en) * | 2012-12-14 | 2013-07-24 | 中山出入境检验检疫局 | Analysis method for tracing import Merlot grape wine production place by using dual finger print |
| CN114324716A (en) * | 2021-08-30 | 2022-04-12 | 华南农业大学 | Method for measuring degree of oxidative rancidity of infant formula rice flour and application of method |
| CN114894917A (en) * | 2022-04-06 | 2022-08-12 | 山东步长制药股份有限公司 | Detection and fingerprint spectrum construction method for volatile components of nardostachys chinensis bunge |
Citations (1)
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| CN101059484A (en) * | 2007-04-14 | 2007-10-24 | 粟学俐 | Use of comprehensive two-dimensional gas chromatography in flavored beer development |
-
2011
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Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101059484A (en) * | 2007-04-14 | 2007-10-24 | 粟学俐 | Use of comprehensive two-dimensional gas chromatography in flavored beer development |
Non-Patent Citations (2)
| Title |
|---|
| R.PERESTRELO.ECT: "《Analytical characterization of the aroma of Tinta Negra Mole red wine:Identification of the main odorants compounds》", 《ANALYTICA CHIMICA ACTA》 * |
| 陶永胜 等: "《中国不同产区赤霞珠干红葡萄酒香气成分数据的可视化分析》", 《分析化学》 * |
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102621193A (en) * | 2012-03-25 | 2012-08-01 | 上海市农业科学院 | Finger-print chromatogram for flavor composition of edible mushroom |
| CN103217487A (en) * | 2012-12-14 | 2013-07-24 | 中山出入境检验检疫局 | Analysis method for tracing import Merlot grape wine production place by using dual finger print |
| CN103217487B (en) * | 2012-12-14 | 2014-10-22 | 中华人民共和国中山出入境检验检疫局 | Analysis method for tracing import Merlot grape wine production place by using dual finger print |
| CN114324716A (en) * | 2021-08-30 | 2022-04-12 | 华南农业大学 | Method for measuring degree of oxidative rancidity of infant formula rice flour and application of method |
| CN114894917A (en) * | 2022-04-06 | 2022-08-12 | 山东步长制药股份有限公司 | Detection and fingerprint spectrum construction method for volatile components of nardostachys chinensis bunge |
| CN114894917B (en) * | 2022-04-06 | 2023-10-20 | 山东步长制药股份有限公司 | Method for detecting volatile components of rhizoma nardostachyos and constructing fingerprint |
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Application publication date: 20111214 |