CN106872599A - A kind of fragrance component in rice to Ningxia carries out the method for separating identification - Google Patents
A kind of fragrance component in rice to Ningxia carries out the method for separating identification Download PDFInfo
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- CN106872599A CN106872599A CN201710112747.XA CN201710112747A CN106872599A CN 106872599 A CN106872599 A CN 106872599A CN 201710112747 A CN201710112747 A CN 201710112747A CN 106872599 A CN106872599 A CN 106872599A
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- 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
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- 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
- G01N30/04—Preparation or injection of sample to be analysed
- G01N30/06—Preparation
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- 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
- G01N30/04—Preparation or injection of sample to be analysed
- G01N30/06—Preparation
- G01N2030/062—Preparation extracting sample from raw material
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Abstract
The invention provides the method that the fragrance component in a kind of rice to Ningxia carries out separating identification, including one using headspace solid-phase microextraction technology separate and enrichment Ningxia rice in flavor substance the step of；One Ningxia 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 for detecting, unknown compound is computed machine examination rope and matches with NIST 14 and NIST 14s spectrums storehouse simultaneously, and composition of the matching degree more than 80% is used as qualitative；Quantitative method compounds content is calculated by internal standard method, i.e., be multiplied by the concentration of TMP as the concentration of compound in sample divided by the ratio of the peak area of TMP using the peak area of various compounds.Authentication method of the invention has the advantages that easy to operate, quick, accurate, applicability is extensive.
Description
Technical field
The invention belongs to analyze detection field, it is related to a kind of method for analyzing fragrance component in rice, specifically one
Plant the method that separation identification is carried out to the fragrance component in the rice of Ningxia.
Background technology
Not only yield is plentiful for Ningxia rice, and because product high-quality is good and famous.Ningxia rice it is complete " grain is round, color is clean,
Glossy, taste is fragrant " four big advantages, and protein, fat content are especially high, are rich in nutritive value.The rice steamed with it, it is pure white such as
Fat, grain sparkling and crystal-clear, viscous and oiliness, the glossy fragrant mouth of grain, can match in excellence or beauty common prosperity with famous Tianjin " small station rice ".Particularly Qingtongxia county leaf
" the big rice of Ye Shengbaipi " of the band of fort one is contained, the polished rice after processing, light reflects semi-transparent, and grain fat is plentiful, even more treasure.
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.
The main oxidation by unrighted acid (linolenic and linoleic etc.) of fragrance component produces, thus content is more, can be used to 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 separate 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 Ningxia
Row separate identification method, the fragrance component in the described this rice to Ningxia carry out separate identification method to solve it is existing
The fragrance component complex steps in the rice of Ningxia are determined in technology and the technical problem such as inaccurate is quantified.
The invention provides the method that the fragrance component in a kind of rice to Ningxia carries out separating identification, including following step
Suddenly：
1) one using headspace solid-phase microextraction technology separate and enrichment Ningxia rice in flavor substance the step of, by Ningxia
Rice is smashed with disintegrating machine, crosses 80 mesh sieves, accurately weighs Ningxia rice sample 5g in the ml headspace bottle of 20mL, adds the μ of 10 μ L 10
The 2 of g/mL, are sealed with silica gel pad immediately after 4,6- trimethylpyridine internal standard compounds, and are balanced at 80 DEG C of water bath with thermostatic control temperature
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 in 2cm on sample at 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) a Ningxia rice flavor substance using Gas chromatographyMass spectrometry detection and analysis obtained by above-mentioned,
And the step of carry out qualitative and quantitative analysis to wherein fragrance component,
A) GC conditions are：Using Rtx-Wax quartz capillary columns, the parameter of the quartzy capillary columns of described Rtx-Wax
It is 30m × 0.25mm × 0.25 μm, carrier gas is helium, and flow is 1.5mL/min, and split sampling, split ratio is set to 10:1, sample introduction
Mouth temperature is 250 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, sweep limits m/z：35-350,260 DEG C of interface temperature；180 DEG C of level Four bar temperature；
3) to detect fragrance component 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 used as qualitative；
4) during quantitative, compounds content is calculated by internal standard method, i.e., removed with the peak area of various compounds
The concentration of TMP as the concentration of compound in sample is multiplied by using the ratio of the peak area of TMP.
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 headspace solid-phase microextraction technology separate and enrichment Ningxia rice in fragrance into
The step of dividing (aldehydes, ketone and alcohols)；One peaceful obtained by above-mentioned using Gas chromatographyMass spectrometry detection and analysis
Summer rice fragrance component (aldehydes, ketone and alcohols), and the step of carry out qualitative and quantitative analysis to wherein fragrance component.
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 in Gas chromatographyMass spectrometry analysis Ningxia rice, fragrance component is qualitative in a set of Ningxia rice of formation
Quantitative analysis method, the authentication method 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 chromatographyMass spectrometry to the perfume (or spice) in the rice of Ningxia
The chromatogram that gas composition is analyzed.
Specific embodiment
The present invention is illustrated below by embodiment, but is not intended to limit the present invention.
It is further explaination using headspace solid-phase microextraction-Gas chromatographyMass spectrometry quick detection and qualitative fixed
The method of the fragrance component in amount Ningxia 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 the rice of Ningxia
Composition carries out qualitative, quantitative, comprises the following steps that：
1) fragrance component in the rice of Ningxia is extracted：
Ningxia rice is smashed with disintegrating machine first, crosses 80 mesh sieves, accurately weigh Ningxia rice sample 5g in the top of 20mL
In empty bottle, sealed with silica gel pad immediately after adding 2,4,6- trimethylpyridine (TMP) internal standard compounds of 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 in 2cm on sample, 30~40min is extracted at 80 DEG C of water bath with thermostatic control temperature, then
It is rapid that extracting head is inserted into gas chromatograph-mass spectrometer (GC-MS) injection port, in 5~6min is desorbed at 250 DEG C, carry out GC-MS analyses.
2) test and analyze step 1 with headspace solid-phase microextraction-Gas chromatographyMass spectrometry) obtained by Ningxia it is big
Fragrance component in rice carries out qualitative and quantitative analysis：
GC conditions：
Using Rtx-Wax quartz capillary column (30m × 0.25mm × 0.25 μm), carrier gas is helium (99.999%), flow
It is 1.5mL/min, split sampling, split ratio is set to 10:1, injector temperature is 250 DEG C, heating schedule：Initial temperature is 40
DEG C, 2min is kept, 240 DEG C are risen to 5 DEG C/min, keep 3min.
Mass Spectrometry Conditions：
Electron impact ion source, electron energy 70eV, ion source temperature is 250 DEG C, using full scan pattern, sweep limits
m/z：35-350,260 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 to match with NIST 14 and NIST 14s spectrums storehouse simultaneously, composition of the matching degree more than 80% is changed as qualification result
Compound content is calculated by internal standard method, i.e., the ratio with the peak area of various compounds divided by the peak area of TMP is multiplied by TMP's
Concentration as compound in sample concentration.
Fragrance component testing result in the inventive method Ningxia rice of table 1.
Claims (3)
1. the fragrance component in a kind of rice to Ningxia carries out the method for separating identification, it is characterised in that comprise the following steps：
1）In the separation of one utilization headspace solid-phase microextraction technology and enrichment Ningxia rice the step of flavor substance, by Ningxia rice
Smashed with disintegrating machine, cross 80 mesh sieves, accurately weigh Ningxia rice sample 5g in the ml headspace bottle of 20 mL, add the μ g/ of 10 μ L 10
The 2 of mL, are sealed with silica gel pad immediately after 4,6- trimethylpyridine internal standard compounds, and are balanced at 80 DEG C of water bath with thermostatic control temperature
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 in 2cm on sample at 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 Ningxia rice flavor substance using Gas chromatographyMass spectrometry detection and analysis obtained by above-mentioned, and it is right
The step of wherein fragrance component carries out qualitative and quantitative analysis,
a）GC conditions are：Using Rtx-Wax quartz capillary columns, the parameter of described Rtx-Wax quartz capillary columns is
30m × 0.25 mm × 0.25 μm, carrier gas is helium, and flow is 1.5mL/min, and split sampling, split ratio is set to 10:1, sample introduction
Mouth temperature is 250 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, sweep limits m/z：35-350,260 DEG C of interface temperature；180 DEG C of level Four bar temperature；
3）During qualitative analysis is carried out to the fragrance component for detecting, unknown compound is computed machine examination rope simultaneously and NIST
14 and NIST 14s spectrums storehouse matches, and composition of the matching degree more than 80% is used as qualitative；
4）During quantitative, compounds content is calculated by internal standard method, i.e., with the peak area of various compounds divided by TMP
The ratio of peak area be multiplied by concentration of the concentration of TMP as compound in sample.
2. the fragrance component in a kind of rice to Ningxia 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 Ningxia according to claim 1 carries out the method for separating identification, its feature
It is：Described quantitative approach is inner mark method ration.
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| CN201710112747.XA CN106872599A (en) | 2017-02-28 | 2017-02-28 | A kind of fragrance component in rice to Ningxia carries out the method for separating identification |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN116990091A (en) * | 2023-09-25 | 2023-11-03 | 黑龙江省农业科学院农产品质量安全研究所 | Rice aroma collection and ingredient determination integrated equipment |
Citations (3)
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| US20070248500A1 (en) * | 2006-04-20 | 2007-10-25 | Janusz Pawliszyn | Internally cooled coated fiber device |
| CN102331466A (en) * | 2011-07-25 | 2012-01-25 | 四川省宜宾五粮液集团有限公司 | Method for comprehensively testing fragrant components of crops |
| CN105572283A (en) * | 2015-12-21 | 2016-05-11 | 南京财经大学 | Analysis method for judging unpolished rice tea aroma quality |
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2017
- 2017-02-28 CN CN201710112747.XA patent/CN106872599A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20070248500A1 (en) * | 2006-04-20 | 2007-10-25 | Janusz Pawliszyn | Internally cooled coated fiber device |
| CN102331466A (en) * | 2011-07-25 | 2012-01-25 | 四川省宜宾五粮液集团有限公司 | Method for comprehensively testing fragrant components of crops |
| CN105572283A (en) * | 2015-12-21 | 2016-05-11 | 南京财经大学 | Analysis method for judging unpolished rice tea aroma quality |
Non-Patent Citations (2)
| Title |
|---|
| ZHI ZENG ET AL.: "Flavor Volatiles of Rice During Cooking Analyzed by Modified Headspace SPME/GC-MS", 《CEREAL CHEM.》 * |
| 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》 * |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN116990091A (en) * | 2023-09-25 | 2023-11-03 | 黑龙江省农业科学院农产品质量安全研究所 | Rice aroma collection and ingredient determination integrated equipment |
| CN116990091B (en) * | 2023-09-25 | 2024-02-13 | 黑龙江省农业科学院农产品质量安全研究所 | Rice aroma collection and ingredient determination integrated equipment |
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