CN106970160A - A kind of fragrance component in rice to the rice fragrance of a flower carries out the method for separating identification - Google Patents
A kind of fragrance component in rice to the rice fragrance of a flower carries out the method for separating identification Download PDFInfo
- Publication number
- CN106970160A CN106970160A CN201710112203.3A CN201710112203A CN106970160A CN 106970160 A CN106970160 A CN 106970160A CN 201710112203 A CN201710112203 A CN 201710112203A CN 106970160 A CN106970160 A CN 106970160A
- Authority
- CN
- China
- Prior art keywords
- rice
- fragrance
- flower
- fragrance component
- qualitative
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
Classifications
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
Landscapes
- Physics & Mathematics (AREA)
- Health & Medical Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Chemical & Material Sciences (AREA)
- Analytical Chemistry (AREA)
- Biochemistry (AREA)
- General Health & Medical Sciences (AREA)
- General Physics & Mathematics (AREA)
- Immunology (AREA)
- Pathology (AREA)
- Other Investigation Or Analysis Of Materials By Electrical Means (AREA)
Abstract
The method for separating identification is carried out the invention provides the fragrance component in a kind of fragrance of a flower meter to rice, including one utilizes the step of headspace solid-phase microextraction technology separates and be enriched with flavor substance in rice fragrance of a flower rice；One rice fragrance of a flower rice flavor substance using the analysis of gas chromatography combined with mass spectrometry technology for detection obtained by above-mentioned, and the step of carry out qualitative and quantitative analysis to wherein fragrance component；During qualitative analysis is carried out to the fragrance component of detection, unknown compound is computed machine examination rope and matched simultaneously with NIST 14 and NIST 14s spectrums storehouse, and composition of the matching degree more than 80% is as qualitative；During one quantitative, compounds content is calculated by internal standard method.TMP concentration is multiplied by as the concentration of compound in sample using the ratio of the peak area of various compounds divided by TMP peak area.The authentication method of the present invention has the advantages that easy to operate, quick, accurate, applicability is extensive.
Description
Technical field
The invention belongs to technical field of analysis and detection, it is related to a kind of method for analyzing fragrance component in rice, specifically
It is that a kind of fragrance component in rice to the rice fragrance of a flower carries out the method for separating identification.
Background technology
Rice fragrance of a flower rice omits sweet tea into food flat flavor, soft slightly to glue, and fragrance is tasty and refreshing, and rice grain surface is glossy gorgeous.Its quality
It is superior, the grain of rice is uniform, bright in color, and mellow long, sweet perfumes are diffused all around, is the good merchantable brand that rice is done in daily life.The rice fragrance of a flower
2- acetyl group -1- the pyrrolins (2-AP) contained in rice have puffed rice fragrance, are the peculiar fragrance of rice, but the material
Testing and appraisal is relatively difficult.
The rice volatile materials detected by Instrumental Analysis is existing 200 kinds, but volatile materials is corresponding with local flavor
Only seldom a part is understood by people in relation.Hexanal (there is grape vinosity), aldehyde C-9 (there is fruit flavor) in rice etc.
Main aoxidized by unrighted acid (linolenic and linoleic etc.) of fragrance component produces, thus content is more, can be for table
Levy rice freshness.The method of traditional detection rice flavor substance is mainly collection, concentration, separation, quantitative, and operating procedure is numerous
It is trivial and separation and quantitative analysis there is certain difficulty.
The content of the invention
For above-mentioned technical problem of the prior art, enter the invention provides the fragrance component in a kind of rice to the rice fragrance of a flower
The method of fragrance component progress separation identification in the method that separation of going is identified, the described this rice to the rice fragrance of a flower will solve existing
The fragrance component complex steps in rice fragrance of a flower rice are determined in technology and the technical problem such as inaccurate is quantified.
The method for separating identification, including following step are carried out the invention provides the fragrance component in a kind of rice to the rice fragrance of a flower
Suddenly：
1) one utilizes the step of headspace solid-phase microextraction technology separates and be enriched with flavor substance in rice fragrance of a flower rice, by rice
Scented rice is smashed with disintegrating machine, crosses 80 mesh sieves, is accurately weighed rice fragrance of a flower rice sample 5g in 20mL ml headspace bottle, is added the μ of 10 μ L 10
Sealed, and balanced at 80 DEG C of water bath with thermostatic control temperature with silica gel pad immediately after the 2 of g/mL, 4,6- trimethylpyridine internal standard compounds
10min, for headspace solid-phase microextraction.Headspace solid-phase microextraction condition is：Extracting head is inserted into ml headspace bottle, and makes extraction
Head extracts 30~40min at 2cm on sample, 80 DEG C of water bath with thermostatic control temperature, then rapid that extracting head is inserted into gas phase color
Spectrum-GC-MS injection port, in 5~6min of desorption at 250 DEG C；
2) one tests and analyzes above-mentioned resulting rice fragrance of a flower rice flavor substance using Gas chromatographyMass spectrometry,
And to wherein fragrance component carry out qualitative and quantitative analysis the step of；
A) GC conditions are：Using the quartzy capillary columns of Rtx-Wax, the parameter of the quartzy capillary columns of described Rtx-Wax
For 30m × 0.25mm × 0.25 μm, carrier gas is helium, and flow is 1.5mL/min, and split sampling, split ratio is set to 20:1, sample introduction
Mouth temperature is 260 DEG C, heating schedule：Initial temperature is 40 DEG C, keeps 2min, and 240 DEG C are risen to 5 DEG C/min, keeps 3min；
B) Mass Spectrometry Conditions are：Electron impact ion source, electron energy 70eV, ion source temperature is 250 DEG C, using full scan
Pattern, scanning range m/z：30-300,250 DEG C of interface temperature；180 DEG C of level Four bar temperature；
3) to the fragrance component of detection carry out qualitative analysis during, unknown compound be computed machine examination rope simultaneously with
NIST 14 and NIST 14s spectrums storehouse matches, and composition of the matching degree more than 80% is as qualitative；
4) during one quantitative, compounds content is calculated by internal standard method.I.e. with the peak face of various compounds
The ratio of product divided by TMP peak area is multiplied by TMP concentration as the concentration of compound in sample.
Further, described analysis and detecting instrument is gas chromatograph-mass spectrometer (GC-MS).
Further, described quantitative approach is inner mark method ration.
The method of the present invention include one using fragrance in the separation of headspace solid-phase microextraction technology and enrichment rice fragrance of a flower rice into
The step of dividing (aldehydes, ketone and alcohols)；One tests and analyzes above-mentioned resulting rice using Gas chromatographyMass spectrometry
The fragrance of a flower rice fragrance component (aldehydes, ketone and alcohols), and to wherein fragrance component carry out qualitative and quantitative analysis the step of.
The present invention is compared with prior art, and its technological progress is significant.The present invention is combined using headspace solid-phase microextraction
Fragrance component is qualitative in fragrance component in Gas chromatographyMass spectrometry analysis rice fragrance of a flower rice, a set of rice fragrance of a flower rice of formation
Quantitative analysis method, authentication method of the invention has the advantages that easy to operate, quick, accurate, applicability is extensive.
Brief description of the drawings
Fig. 1 is that embodiment 1 uses headspace solid-phase microextraction-gas-chromatography-nitrogen phosphorous detector-mass spectrometric hyphenated technique to rice
The chromatogram that fragrance component in scented rice is analyzed.
Embodiment
The present invention is illustrated below by embodiment, but is not intended to limit the present invention.
Quickly examined using headspace solid-phase microextraction-gas-chromatography-nitrogen phosphorous detector-mass spectrometric hyphenated technique for further explaination
The method for the fragrance component surveyed in simultaneously qualitative, quantitative rice fragrance of a flower rice, is described in more detail with reference to example.
Embodiment 1
This method is mainly using headspace solid-phase microextraction-Gas chromatographyMass spectrometry to the fragrance in rice fragrance of a flower rice
Composition carries out qualitative, quantitative, comprises the following steps that：
1) fragrance component in rice fragrance of a flower rice is extracted：
Rice fragrance of a flower rice is smashed with disintegrating machine first, 80 mesh sieves are crossed, rice fragrance of a flower rice sample 5g is accurately weighed in 20mL top
In empty bottle, sealed immediately with silica gel pad after 2,4,6- trimethylpyridine (TMP) internal standard compounds for adding the μ g/mL of 10 μ L 10, and
10min is balanced at 80 DEG C of water bath with thermostatic control temperature, for headspace solid-phase microextraction.Headspace solid-phase microextraction condition is：By extracting head
It is inserted into ml headspace bottle, and extracting head is at 2cm on sample, 80 DEG C of water bath with thermostatic control temperature and extract 30~40min, then
It is rapid that extracting head is inserted into gas chromatograph-mass spectrometer (GC-MS) injection port, in desorbing 5~6min at 250 DEG C, carry out GC-MS analyses.
2) with headspace solid-phase microextraction-Gas chromatographyMass spectrometry detection and analysis step 1) obtained by the rice fragrance of a flower
Fragrance component in rice carries out qualitative and quantitative analysis：
GC conditions：
Using the quartzy capillary columns (30m × 0.25mm × 0.25 μm) of Rtx-Wax, carrier gas is helium (99.999%), flow
For 1.5mL/min, split sampling, split ratio is set to 20:1, injector temperature is 260 DEG C, heating schedule：Initial temperature is 40
DEG C, 2min is kept, 240 DEG C are risen to 5 DEG C/min, 3min is kept.
Mass Spectrometry Conditions：
Electron impact ion source, electron energy 70eV, ion source temperature is 250 DEG C, using full scan pattern, scanning range
m/z：30-300,250 DEG C of interface temperature；180 DEG C of level Four bar temperature.
3) qualitative and quantitative of material is detected：GC-MS data processings are completed by Shimadzu software systems, and unknown compound is through meter
Calculate machine examination rope simultaneously with NIST 14 and NIST 14s spectrums storehouse to match, composition of the matching degree more than 80% is changed as qualification result
Compound content is calculated by internal standard method, i.e., be multiplied by TMP's with the ratio of the peak area of various compounds divided by TMP peak area
Concentration as compound in sample concentration.
Fragrance component testing result in the inventive method rice fragrance of a flower rice of table 1.
Claims (3)
1. the fragrance component in a kind of rice to the rice fragrance of a flower carries out the method for separating identification, it is characterised in that comprise the following steps：
1）One utilizes the step of headspace solid-phase microextraction technology separates and be enriched with flavor substance in rice fragrance of a flower rice, by rice fragrance of a flower rice
Smashed with disintegrating machine, cross 80 mesh sieves, accurately weighed rice fragrance of a flower rice sample 5g in 20 mL ml headspace bottle, add the μ g/ of 10 μ L 10
Sealed, and balanced at 80 DEG C of water bath with thermostatic control temperature with silica gel pad immediately after the 2 of mL, 4,6- trimethylpyridine internal standard compounds
10min, for headspace solid-phase microextraction；Headspace solid-phase microextraction condition is：Extracting head is inserted into ml headspace bottle, and makes extraction
Head extracts 30~40min at 2cm on sample, 80 DEG C of water bath with thermostatic control temperature, then rapid that extracting head is inserted into gas phase color
Spectrum-GC-MS injection port, in 5~6min of desorption at 250 DEG C；
2）One tests and analyzes above-mentioned resulting rice fragrance of a flower rice flavor substance using Gas chromatographyMass spectrometry, and right
The step of wherein fragrance component carries out qualitative and quantitative analysis；
a）GC conditions are：Using the quartzy capillary columns of Rtx-Wax, the parameter of the quartzy capillary columns of described Rtx-Wax is
Mm × 0.25 μm of 30m × 0.25, carrier gas is helium, and flow is 1.5mL/min, and split sampling, split ratio is set to 20:1, sample introduction
Mouth temperature is 260 DEG C, heating schedule：Initial temperature is 40 DEG C, keeps 2min, and 240 DEG C are risen to 5 DEG C/min, keeps 3min；
b）Mass Spectrometry Conditions are：Electron impact ion source, electron energy 70eV, ion source temperature is 250 DEG C, using full scan mould
Formula, scanning range m/z：30-300,250 DEG C of interface temperature；180 DEG C of level Four bar temperature；
3）During qualitative analysis is carried out to the fragrance component of detection, unknown compound is computed machine examination rope while and NIST
14 and NIST 14s spectrums storehouse matches, and composition of the matching degree more than 80% is as qualitative；
4）During one quantitative, compounds content is calculated by internal standard method；Removed with the peak area of various compounds
TMP concentration is multiplied by as the concentration of compound in sample using the ratio of TMP peak area.
2. the fragrance component in a kind of rice to the rice fragrance of a flower according to claim 1 carries out the method for separating identification, its feature
It is：Described analysis and detecting instrument is gas chromatograph-mass spectrometer (GC-MS).
3. the fragrance component in a kind of rice to the rice fragrance of a flower according to claim 1 carries out the method for separating identification, its feature
It is：Described quantitative approach is inner mark method ration.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201710112203.3A CN106970160A (en) | 2017-02-28 | 2017-02-28 | A kind of fragrance component in rice to the rice fragrance of a flower carries out the method for separating identification |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201710112203.3A CN106970160A (en) | 2017-02-28 | 2017-02-28 | A kind of fragrance component in rice to the rice fragrance of a flower carries out the method for separating identification |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN106970160A true CN106970160A (en) | 2017-07-21 |
Family
ID=59328802
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201710112203.3A Pending CN106970160A (en) | 2017-02-28 | 2017-02-28 | A kind of fragrance component in rice to the rice fragrance of a flower carries out the method for separating identification |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN106970160A (en) |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108828107A (en) * | 2018-09-04 | 2018-11-16 | 浙江公正检验中心有限公司 | A kind of gas chromatography combined with mass spectrometry method detecting the scented rice true and false |
| CN112114049A (en) * | 2019-06-19 | 2020-12-22 | 天津科技大学 | Quantitative detection method for main aroma component 2-acetyl-1-pyrroline in fragrant rice |
| CN114019046A (en) * | 2021-10-31 | 2022-02-08 | 浙江农林大学 | Technical method for judging eating quality of paddy based on volatile components of paddy |
| CN116183786A (en) * | 2022-12-12 | 2023-05-30 | 中国农业科学院烟草研究所(中国烟草总公司青州烟草研究所) | Identification method for trace glutinous rice aroma characteristic key aroma compound in tobacco |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20070248500A1 (en) * | 2006-04-20 | 2007-10-25 | Janusz Pawliszyn | Internally cooled coated fiber device |
-
2017
- 2017-02-28 CN CN201710112203.3A patent/CN106970160A/en active Pending
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20070248500A1 (en) * | 2006-04-20 | 2007-10-25 | Janusz Pawliszyn | Internally cooled coated fiber device |
Non-Patent Citations (6)
| Title |
|---|
| MAOMAO ZENG ET AL.: "Determination of flavor components of rice bran by GC-MS and chemometrics", 《ANALYTICAL METHODS》 * |
| ZHI ZENG ET AL.: "Flavor Volatiles of Rice During Cooking Analyzed by Modified Headspace SPME/GC-MS", 《CEREAL CHEM.》 * |
| 刘国诠 等: "《色谱柱技术》", 31 July 2001, 化学工业出版社 * |
| 刘美艳 等: "酶法方便米饭香气成分的SPME/GC-MS分析", 《食品科学》 * |
| 孙谦 等: "固相微萃取-气相色谱-质谱联用快速鉴别香米真伪", 《食品安全质量检测学报》 * |
| 林家永 等: "顶空固相微萃取-气质联用法分析稻谷挥发性成分", 《食品科学》 * |
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108828107A (en) * | 2018-09-04 | 2018-11-16 | 浙江公正检验中心有限公司 | A kind of gas chromatography combined with mass spectrometry method detecting the scented rice true and false |
| CN112114049A (en) * | 2019-06-19 | 2020-12-22 | 天津科技大学 | Quantitative detection method for main aroma component 2-acetyl-1-pyrroline in fragrant rice |
| CN114019046A (en) * | 2021-10-31 | 2022-02-08 | 浙江农林大学 | Technical method for judging eating quality of paddy based on volatile components of paddy |
| CN116183786A (en) * | 2022-12-12 | 2023-05-30 | 中国农业科学院烟草研究所(中国烟草总公司青州烟草研究所) | Identification method for trace glutinous rice aroma characteristic key aroma compound in tobacco |
| CN116183786B (en) * | 2022-12-12 | 2023-10-10 | 中国农业科学院烟草研究所(中国烟草总公司青州烟草研究所) | Identification method for trace glutinous rice aroma characteristic key aroma compound in tobacco |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| Wang et al. | Uncover the flavor code of strong-aroma baijiu: Research progress on the revelation of aroma compounds in strong-aroma baijiu by means of modern separation technology and molecular sensory evaluation | |
| CN104267112B (en) | A kind of method of real-time analysis xeres aroma component | |
| CN106970160A (en) | A kind of fragrance component in rice to the rice fragrance of a flower carries out the method for separating identification | |
| Verzera et al. | Fast quantitative determination of aroma volatile constituents in melon fruits by headspace–solid-phase microextraction and gas chromatography–mass spectrometry | |
| CN106053628A (en) | Method for rapidly determining fragrance components of tea quantitatively and qualitatively | |
| CN100432668C (en) | Method for determining volatile element in shaoxing wine | |
| Capobiango et al. | Identification of aroma-active volatiles in banana Terra spirit using multidimensional gas chromatography with simultaneous mass spectrometry and olfactometry detection | |
| CN104316635A (en) | Method for rapidly identifying flavor and quality of fruits | |
| Wang et al. | Comparison of volatile compositions of 15 different varieties of Chinese jujube (Ziziphus jujuba Mill.) | |
| CN110261526A (en) | A kind of tomato flavor quality determination method based on tomato odor characteristic compound | |
| CN115060814B (en) | Method for rapidly identifying rose tea in different drying modes | |
| CN108845041A (en) | A kind of detection method measuring redwood volatilization and half volatile chemical component | |
| CN108181411A (en) | A kind of passionflower aroma substance detection method | |
| CN114235981A (en) | Method for identifying perilla leaf essential oil by combining gas-mass spectrometry-sniffing instrument and gas chromatography-ion mobility spectrometry | |
| CN106940349A (en) | A kind of fragrance component in oily glutinous rice carries out the method for separating identification | |
| CN107014913A (en) | A kind of fragrance component in Moli rice carries out the method for separating identification | |
| CN113049722A (en) | Construction method and application of volatile aroma substance fingerprint spectrum | |
| CN109470779A (en) | The construction method and identification application of a kind of natural middle bee honey of lychee flowers and natural Apis mellifera honey of lychee flowers finger-print | |
| CN107179375A (en) | A kind of method of volatile flavor substance in ultrasonic method auxiliary measuring brown rice | |
| CN106198804A (en) | The authentication method of nitrogen-containing compound in a kind of cherry wine | |
| CN106872599A (en) | A kind of fragrance component in rice to Ningxia carries out the method for separating identification | |
| CN110514757A (en) | A kind of method of Volatile flavor components in fast resolving white wine | |
| CN107462624A (en) | The rapid assay methods of main ester type compound content in a kind of white wine base liquor | |
| CN106908535A (en) | A kind of fragrance component in scented rice to peach blossom carries out the method for separating identification | |
| CN102279230A (en) | Method for establishing volatile ingredient fingerprint map of agricultural product and processed product of agricultural product |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| RJ01 | Rejection of invention patent application after publication |
Application publication date: 20170721 |
|
| RJ01 | Rejection of invention patent application after publication |