CN109324124A - The detection method of difference small-molecule substance in efficient identification xanthochromia and normal paddy - Google Patents
The detection method of difference small-molecule substance in efficient identification xanthochromia and normal paddy Download PDFInfo
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- CN109324124A CN109324124A CN201810692960.7A CN201810692960A CN109324124A CN 109324124 A CN109324124 A CN 109324124A CN 201810692960 A CN201810692960 A CN 201810692960A CN 109324124 A CN109324124 A CN 109324124A
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- 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
- G01N30/96—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 using ion-exchange
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Abstract
The invention belongs to field of food detection, more particularly to a kind of detection method of difference small-molecule substance in efficient identification xanthochromia and normal paddy, include the following steps: 1) to utilize automatic headspace sampling unit, by way of increasing temperature, balanced gas environment evaporates the flavor substance in determinand effectively；2) volatile materials is detected by gas phase-ion mobility spectrometry；3) GC × IMS Library Search software is utilized, the NIST database and ims database built in application software can carry out qualitative analysis to substance.The present invention utilizes the advanced technology of GC-IMS, carries out extraction detection and qualitative to the volatile component in xanthochromia paddy.Result of study shows that the present invention can quickly analyze the volatile materials in xanthochromia and normal paddy by GC-IMS technology.
Description
Technical field
The invention belongs to field of food detection, and in particular to difference small molecule in a kind of efficient identification xanthochromia and normal paddy
The detection method of substance.
Background technique
Paddy xanthochromia is the major issue that paddy industry faces, and color is rice an important factor for determining paddy quality
Paddy xanthochromia can reduce its nutritive value and commercial value, bring extreme loss to paddy industry.The rotten most important characteristics of paddy
One of be exactly to generate bad perfume compound, drying mode, stored manner, storage ambient etc. after the growing environment of paddy, harvest
Factor can all influence the variation of the type and content of volatile materials in paddy.But the current stage, there is no detect xanthochromia rice
The effective means of paddy volatile component variation.
Summary of the invention
The purpose of the present invention is to overcome the defects in the prior art, provides in a kind of efficient identification xanthochromia and normal paddy
The detection method of difference small-molecule substance.
The present invention to achieve the above object, using following technical scheme:
The detection method of difference small-molecule substance in a kind of efficient identification xanthochromia and normal paddy, which is characterized in that including
Following step:
1) automatic headspace sampling unit is utilized, by way of increasing temperature, balanced gas environment makes the flavor in polished rice
Substance effectively evaporates；
2) volatile materials is detected by gas phase-ion mobility spectrometry；
3) GC × IMS Library Search software, NIST database and IMS database built in application software are utilized
Qualitative analysis can be carried out to substance
Parameter is arranged in the sample introduction of automatic headspace sampling unit in step 1) are as follows: 3-20g polished rice is taken to extract in 10-40mL head space
It takes in bottle, the temperature setting of automatic headspace sampling unit is 60 DEG C -95 DEG C, equilibration time 10min-30min, sample introduction needle temperature
Degree is 98 DEG C, balancing speed 500rpm, and sampling volume is 500 μ L.
Gas phase-ion mobility spectrometry setting parameter in step 2) are as follows: spectrum column type is FS-SE-54-CB-0.5, column length
15m, internal diameter: 0.53mm；40 DEG C of column temperature, IMS temperature 45 C, carrier gas/drift gas is N2, analysis time 15min.
Compared with prior art, the beneficial effects of the present invention are:
At present to the research in paddy xanthochromia field, the storage ambients such as temperature and humidity, bacterial fungus and its metabolite are concentrated on
Etc. the effect that is played during paddy xanthochromia of factors and the variation of physical and chemical index of xanthochromia paddy etc., and for Huang
Becoming the researchs such as the composition variation of volatile component in paddy, there is not been reported.
The present invention utilizes the advanced technology of GC-IMS, carries out extraction detection to the volatile component in xanthochromia paddy and determines
Property.Result of study shows that the present invention can quickly analyze the volatile materials in xanthochromia and normal paddy by GC-IMS technology；It is logical
GC separation is crossed with the secondary separation of IMS, it can be achieved that volatile materials it is quick and precisely qualitative.It is a kind of accurate, quick, operation letter
Just detection xanthochromia and normal paddy in difference volatile materials effective means, the present invention cannot be only used for polished rice volatility at
The detection divided can be also used for the volatile materials of detection rice, the flavor substance variation during foodstuff preservation be detected, to grain
Monitoring is played the role of in the flavor substance variation eaten in storage, may finally establish the Early-warning Model of paddy xanthochromia mechanism.
Detailed description of the invention
Fig. 1 is the comparison diagram of the xanthochromia and normal paddy volatile materials using LAV flavor analysis software detection glutinous rice；
Fig. 2 is the comparison diagram of the xanthochromia and normal paddy volatile materials using LAV flavor analysis software detection japonica rice；
Fig. 3 is that 2 glutinous rice of comparative example normally organizes the result pair analyzed with the volatile organic matter after 4 xanthochromia group cooking rice of embodiment
Than figure；
Fig. 4 is the Comparative result of the volatile organic matter analysis of 5 polished rice rice yellowed rice of embodiment and the normal rice of comparative example 3
Figure.
Specific embodiment
In order to make those skilled in the art more fully understand technical solution of the present invention, with reference to the accompanying drawing and most
The present invention is described in further detail for good embodiment.
Embodiment 1:
1) it takes 10g xanthochromia glutinous rice in 30mL headspace extraction bottle, carries out headspace solid-phase microextraction；Wherein automatic headspace sampling
The temperature setting of unit is 70 DEG C, equilibration time 15min, and sample introduction needle temperature is 98 DEG C, balancing speed 500rpm.
2) after the completion of extracting, it is immediately inserted into automatic sampling needle, sampling volume is 500 μ L；The chromatography of GC-IMS in step 3)
Column type is FS-SE-54-CB-0.5, column length 15m, internal diameter: 0.53mm；40 DEG C of column temperature, IMS temperature 45 C, carrier gas/drift gas
For N2, analysis time 15min.
3) GC × IMS Library Search software is utilized, to the qualitative by software of unknown volatile component each in sample
Built-in NIST database and ims database acquire；Peak volume indicates to obtain the opposite of each volatile component in derived data
Content.
Embodiment 2: the difference of embodiment 2 and embodiment 1 is only that the sample introduction of automatic headspace sampling unit in step 1) is set
It sets parameter difference: taking 3g polished rice in 10mL headspace extraction bottle, the temperature setting of automatic headspace sampling unit is 60 DEG C, when balance
Between be 10min, sample introduction needle temperature be 98 DEG C, balancing speed 500rpm, sampling volume be 500 μ L.
Embodiment 3: the difference of embodiment 3 and embodiment 1 is only that the sample introduction of automatic headspace sampling unit in step 1) is set
It sets parameter difference: taking 20g polished rice in 40mL headspace extraction bottle, the temperature setting of automatic headspace sampling unit is 95 DEG C, balance
Time is 30min, and sample introduction needle temperature is 98 DEG C, balancing speed 500rpm, and sampling volume is 500 μ L.
Embodiment 4: embodiment 4 is same as Example 1, and difference is only that, determinand is after the shelling of xanthochromia glutinous rice is removed the peel
Polished rice, boiling at rice carry out volatile materials detection.
Embodiment 5: embodiment 5 is same as Example 1, and difference is only that, determinand is after the shelling of xanthochromia polished rice is removed the peel
Polished rice, boiling at rice carry out volatile materials detection.
Embodiment 6: embodiment 6 is same as Example 1, and difference is only that, determinand is xanthochromia polished rice.
Comparative example 1: the difference of comparative example 1 and embodiment 1, which is only that, is changed to normal glutinous rice for xanthochromia glutinous rice.
Comparative example 2: the difference of comparative example 2 and embodiment 4, which is only that, is changed to normal glutinous rice for xanthochromia glutinous rice.
Comparative example 3: the difference of comparative example 3 and embodiment 5, which is only that, is changed to normal polished rice for xanthochromia polished rice.
Comparative example 4: the difference of comparative example 1 and embodiment 6, which is only that, is changed to normal polished rice for xanthochromia polished rice.
Fig. 1 is the picture of the xanthochromia and normal paddy volatile materials using LAV flavor analysis software detection glutinous rice, left side
It is the volatile materials picture of the normal rice of glutinous rice, right side is the volatile materials picture of glutinous rice yellowed rice.Ordinate represents in figure
The retention time of gas-chromatography, abscissa represent the Ion transfer time, at abscissa 8.0 grey vertical line be the peak RIP (react from
Sub- peak), each point of the peak RIP two sides represents a kind of volatile organic matter.The background of entire figure is black, the face of the point of appearance
Color is different, and the concentration of representative species is different, and white indicates that concentration is lower, and grey indicates that concentration is higher, and color, which is more deeply felt, shows concentration
It is bigger.
Table 1 is the difference substance of 1 glutinous rice yellowed rice of embodiment Yu the normal glutinous rice of comparative example 1, utilizes GC × IMS Library
Search software, what NIST database and ims database built in application software were organized to the glutinous rice xanthochromia group detected and normally
Otherness volatile materials carries out the information of qualitative analysis, including title, No. CAS, retention index, retention time, Ion transfer
The information such as time, different sample peak volumes, the peak volume of each substance is different, represents the substance and has differences in different sample rooms.
Table 1
Raw material are as follows for the shelling xanthochromia of polished rice and the detection of normal paddy volatile materials: Fig. 2 is to utilize LAV flavor
Analyze the xanthochromia of software detection japonica rice and the picture of normal paddy volatile materials；Left side is the volatile materials of the normal rice of polished rice
Picture, right side are the volatile materials pictures of polished rice yellowed rice.
The difference substance of 2 embodiment of table, 6 polished rice yellowed rice and the normal polished rice of comparative example 4 is to utilize GC × IMS Library
Search software, the difference substance of NIST database and ims database built in application software to polished rice yellowed rice and normal rice
Carry out the information of qualitative analysis, including title, No. CAS, retention index, retention time, transit time, different sample peak volume etc.
The peak volume of information, each substance is different, represents the substance and has differences in different sample rooms.
Table 2
Table 3 is the information of the difference substance progress qualitative analysis of 4 glutinous rice rice yellowed rice of embodiment and the normal rice of comparative example 2
As a result, Fig. 3 be normally organized for 2 glutinous rice of comparative example with after 4 xanthochromia group cooking rice of embodiment volatile organic matter analyze, lead to
Cross the peak volume of more each substance, it can be determined that sample room whether there is difference.
Table 3
Table 4 is the letter of the difference substance progress qualitative analysis of 5 polished rice rice yellowed rice of embodiment and the normal rice of comparative example 3
Breath, Fig. 4 is normally to organize to analyze with the volatile organic matter after xanthochromia group cooking rice for polished rice, by comparing the peak body of each substance
Product, it can be determined that sample room whether there is difference.
Table 4
The above is only a preferred embodiment of the present invention, for those of ordinary skill in the art, according to the present invention
Thought, there will be changes in the specific implementation manner and application range, and the content of the present specification should not be construed as to the present invention
Limitation.
Claims (3)
1. the detection method of difference small-molecule substance in a kind of efficient identification xanthochromia and normal paddy, which is characterized in that including under
State step:
1) automatic headspace sampling unit is utilized, by way of increasing temperature, balanced gas environment makes the flavor in determinand
Matter effectively evaporates；
2) volatile materials is detected by gas phase-ion mobility spectrometry；
3) GC × IMS Library Search software is utilized, NIST database and ims database built in application software can be right
Substance carries out qualitative analysis.
2. the detection method of difference small-molecule substance in efficient identification xanthochromia according to claim 1 and normal paddy,
It is characterized in that, parameter is arranged in the sample introduction of automatic headspace sampling unit in step 1) are as follows: 3-20g polished rice is taken to extract in 10-40mL head space
It takes in bottle, the temperature setting of automatic headspace sampling unit is 60 DEG C -95 DEG C, equilibration time 10min-30min, sample introduction needle temperature
It is 98 DEG C, balancing speed 500rpm, sampling volume is 500 μ L.
3. the detection method of difference small-molecule substance in efficient identification xanthochromia according to claim 1 and normal paddy,
It is characterized in that, gas phase-ion mobility spectrometry setting parameter in step 2) are as follows: spectrum column type is FS-SE-54-CB-0.5, column length
15m, internal diameter: 0.53mm；40 DEG C of column temperature, IMS temperature 45 C, carrier gas/drift gas is N2, analysis time 15min.
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Cited By (5)
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| CN110441423A (en) * | 2019-08-08 | 2019-11-12 | 山东省粮油检测中心 | A kind of method and its system measuring grain fragrance component |
| CN111948321A (en) * | 2020-08-20 | 2020-11-17 | 中国农业大学 | Method for evaluating aroma components of millets of different varieties based on gas phase ion mobility spectrometry |
| CN113390980A (en) * | 2021-05-24 | 2021-09-14 | 中国农业科学院农产品加工研究所 | Method for evaluating flavor substance change in pancake processing |
| CN114813975A (en) * | 2021-01-19 | 2022-07-29 | 南京财经大学 | Detection method for efficiently identifying grain storage pests in paddy |
| CN114813977A (en) * | 2021-01-19 | 2022-07-29 | 南京财经大学 | Method for nondestructive testing of corn elephant in rice by using odor fingerprint spectrum |
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Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110441423A (en) * | 2019-08-08 | 2019-11-12 | 山东省粮油检测中心 | A kind of method and its system measuring grain fragrance component |
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| CN111948321A (en) * | 2020-08-20 | 2020-11-17 | 中国农业大学 | Method for evaluating aroma components of millets of different varieties based on gas phase ion mobility spectrometry |
| CN114813975A (en) * | 2021-01-19 | 2022-07-29 | 南京财经大学 | Detection method for efficiently identifying grain storage pests in paddy |
| CN114813977A (en) * | 2021-01-19 | 2022-07-29 | 南京财经大学 | Method for nondestructive testing of corn elephant in rice by using odor fingerprint spectrum |
| CN114813977B (en) * | 2021-01-19 | 2023-05-12 | 南京财经大学 | Method for nondestructive detection of corn images in rice by using odor fingerprint |
| CN114813975B (en) * | 2021-01-19 | 2023-08-08 | 南京财经大学 | Detection method for efficiently identifying grain storage pests in rice |
| CN113390980A (en) * | 2021-05-24 | 2021-09-14 | 中国农业科学院农产品加工研究所 | Method for evaluating flavor substance change in pancake processing |
| CN113390980B (en) * | 2021-05-24 | 2023-08-25 | 中国农业科学院农产品加工研究所 | Evaluation method for flavor substance change in pancake processing |
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Application publication date: 20190212 |