CN114858937A - Method for identifying Xinjiang 'warm 185' thin-skinned fresh walnuts - Google Patents
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- 239000012159 carrier gas Substances 0.000 claims description 6
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- 229910052757 nitrogen Inorganic materials 0.000 claims description 6
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- GBMDVOWEEQVZKZ-UHFFFAOYSA-N methanol;hydrate Chemical compound O.OC GBMDVOWEEQVZKZ-UHFFFAOYSA-N 0.000 claims description 3
- PNJWIWWMYCMZRO-UHFFFAOYSA-N pent‐4‐en‐2‐one Natural products CC(=O)CC=C PNJWIWWMYCMZRO-UHFFFAOYSA-N 0.000 claims description 3
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- OBNCKNCVKJNDBV-UHFFFAOYSA-N butanoic acid ethyl ester Natural products CCCC(=O)OCC OBNCKNCVKJNDBV-UHFFFAOYSA-N 0.000 abstract 2
- WEVYAHXRMPXWCK-UHFFFAOYSA-N Acetonitrile Chemical compound CC#N WEVYAHXRMPXWCK-UHFFFAOYSA-N 0.000 description 3
- 239000010903 husk Substances 0.000 description 3
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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
- G01N30/96—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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- Analytical Chemistry (AREA)
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- General Health & Medical Sciences (AREA)
- General Physics & Mathematics (AREA)
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Abstract
The invention discloses a method for identifying Xinjiang 'warm 185' thin-skinned fresh walnuts, which comprises the following steps: measuring the content of arbutin in the green peel of the 'warm 185' thin-skinned walnut by adopting a liquid chromatography, wherein the content is required to reach 100-150 mug/g; the characteristic flavor substances in the fresh kernel are determined by gas phase ion mobility chromatography, and the fresh walnut kernel is required to contain 29 characteristic flavor substances such as propionaldehyde, isopropanol (monomer), isopropanol (dimer), trans-2, 4-heptadienal, isoamyl acetate (monomer), isoamyl acetate (dimer), propyl acetate, 2-methyl butanol (monomer), 2-methyl butanol (dimer), isobutyl acetate, 3-hydroxy ethyl butyrate (monomer), 3-hydroxy ethyl butyrate (dimer), 3-hydroxy-2-butanone (monomer), 3-hydroxy-2-butanone (dimer) and the like. The method can accurately realize the identification of the 'warm 185' thin-skinned fresh walnuts.
Description
Technical Field
The invention relates to the field of agriculture, in particular to a method for identifying Xinjiang 'warm 185' thin-skinned fresh walnuts.
Background
The thin-skin walnut is one of representative special forest fruits in Xinjiang, the thin-skin walnut represented by 'Wen 185' is very popular with consumers at home and abroad due to the characteristics of attractive appearance, thin shell, delicious taste, unique flavor and the like, more than 70% of the current market is consumed in a dry form, the thin-skin walnut is defined and identified mainly from the thickness (less than or equal to 1.0mm) of the shell of the dry fruit, and the identification standard or method of other related characteristic components is lacked. With the enhancement of health care consciousness of consumers, Xinjiang thin-skin fresh walnuts become a 'new favorite' sold in the market at different peaks in recent years, but the phenomenon of being fake and genuine and being secondary and good exists in production, so that the market cognition on the Xinjiang thin-skin fresh walnut brand is influenced, and the healthy development of the fresh thin-skin walnut postpartum industry which is just aroused is directly restrained. Therefore, the research and development of the specific index and the identification method of Xinjiang 'warm 185' thin-skin fresh walnuts have very important practical significance.
Disclosure of Invention
In order to solve the problems, the invention provides a method for identifying Xinjiang 'warm 185' thin-skin fresh walnuts, which can accurately identify the 'warm 185' thin-skin fresh walnuts.
In order to achieve the purpose, the invention adopts the technical scheme that:
a method for identifying Xinjiang 'warm 185' thin-skinned fresh walnuts is characterized by comprising the following steps: the method comprises the following steps:
s1, measuring the arbutin content in the 'warm 185' thin-skinned walnut green peel by adopting a liquid chromatography, wherein the arbutin content is required to reach 100-150 mug/g;
s2, determining characteristic flavor substances in fresh kernel by gas phase ion mobility chromatography, wherein fresh walnut kernel is required to contain propionaldehyde, isopropanol (monomer), isopropanol (dimer), trans-2, 4-heptadienal, isoamyl acetate (monomer), isoamyl acetate (dimer), propyl acetate, 2-methylbutanol (monomer), 2-methylbutanol (dimer), isobutyl acetate, ethyl 3-hydroxybutyrate (monomer), ethyl 3-hydroxybutyrate (dimer), 3-hydroxy-2-butanone (monomer), 3-hydroxy-2-butanone (dimer), ethyl acrylate, acetic acid (monomer), acetic acid (dimer), isopropyl acetate (monomer), isopropyl acetate (dimer), 2-methylbutanal, and isopropyl acetate (monomer), N-butyraldehyde, 2-butanone (monomer), 2-butanone (dimer), 2-methylacrolein, n-hexanal, 3-pentanone, 2-hexanone, 3-hydroxy-2-butanone, 3-methyl-2-butenal.
As a further design of the present solution, step S1 specifically includes the following steps:
accurately weighing 3g of fresh walnut jelly, adding 80% methanol water according to the material-liquid ratio of 1:10 into a 15ml brown centrifuge tube, uniformly mixing for 5min by oscillation, carrying out ultrasonic extraction for 30min, and centrifuging for 15min at 4000 r/min. Transferring the supernatant into another centrifuge tube, repeatedly extracting for 2 times, mixing the supernatants for 3 times, reducing the pressure of nitrogen at room temperature to dryness, dissolving with 20% acetonitrile water to constant volume of 10ml, shaking, mixing, and filtering with 0.45 μm filter membrane to be detected; and (3) testing conditions are as follows: c 18 A chromatographic column: 250 × 4.6mm, column temperature: 30 degrees; sample introduction amount: 20 ul; wavelength: 254 nm; methanol: 0.2% phosphoric acid water isocratic elution 45: 55; flow rate: 1 ml/min.
As a further design of the present solution, step S2 specifically includes the following steps
Weighing 3.00g of crushed fresh nucleolus sample, placing the crushed fresh nucleolus sample into a 20mL headspace sample injection bottle for incubation, extracting headspace components in the bottle by using a heated sample injection needle, and analyzing volatile components by using a Flavour Spec gas phase ion mobility spectrometer; wherein, the GC-IMS determination conditions are as follows: the headspace incubation temperature is 50 ℃, the incubation time is 10min, and the incubation rotation speed is 500 r/min; the carrier gas is high-purity nitrogen (not less than 99.999%), the temperature of the chromatographic column is 40 ℃, the chromatographic operation time is 20min, the flow rate gradient of the carrier gas is set to be 2.00mL/min and kept for 2min, the flow rate gradient is linearly increased to 20.00mL/min within 6min, and the flow rate gradient is linearly increased to 100.00mL/min within 2min and kept for 5 min; the headspace sampling needle temperature is 55 ℃, the sampling amount is 500 mu L, the non-shunting mode is adopted, and the cleaning time is 0.50 min. And (3) data analysis: analyzing the spectrum by adopting LAV (laboratory Analytical viewer) software, and constructing a difference map and a fingerprint map of the volatile organic compounds by adopting a Reporter and a Gallery plug-in program; the software is internally provided with an NIST database and an IMS database to carry out qualitative analysis on the substances.
In the scheme, the identification of the 'warm 185' thin-shelled fresh walnuts can be accurately realized by taking the content requirement of arbutin in the 'warm 185' thin-shelled fresh walnut green husks and 29 unique characteristic flavor substances in the walnut kernels as identification indexes.
Drawings
Other features, objects and advantages of the invention will become more apparent upon reading of the detailed description of non-limiting embodiments with reference to the following drawings:
FIG. 1 is a map of arbutin standard.
FIG. 2 is a map of arbutin standard in 'Wen 185' thin-skinned fresh walnut green husk.
FIG. 3 is a gas phase ion mobility spectrum of 'warm 185' thin-skinned fresh walnut.
FIG. 4 is a characteristic flavor map of 'Wen 185' thin-skinned fresh walnuts, which is particularly different from other fresh walnut varieties.
Detailed Description
The present invention will be described in detail with reference to specific examples. The following examples will assist those skilled in the art in further understanding the invention, but are not intended to limit the invention in any way. It should be noted that variations and modifications can be made by persons skilled in the art without departing from the spirit of the invention. All falling within the scope of the present invention.
Example 1
The method for identifying the Xinjiang 'warm 185' thin-skinned fresh walnuts in the embodiment mainly identifies the Xinjiang 'warm 185' thin-skinned fresh walnuts from two aspects, on one hand, the method adopts a liquid chromatography method to measure the content of arbutin in the green husks of the 'warm 185' thin-skinned walnuts, and the content is required to reach 100-150 mug/g (see figure 1); specifically, 3g of fresh walnut jelly sample is accurately weighed and separated in 15ml of brownAdding 80% methanol water into the core tube according to the feed-liquid ratio of 1:10, shaking and mixing uniformly for 5min, performing ultrasonic extraction for 30min, and centrifuging at 4000r/min for 15 min. Transferring the supernatant to another centrifuge tube, repeatedly extracting for 2 times, combining 3 times of supernatants, and decompressing to dryness under nitrogen at room temperature. Finally, dissolving the mixture with 20 percent acetonitrile to a constant volume of 10ml, shaking and mixing the mixture evenly, and filtering the mixture through a 0.45 mu m filter membrane to be detected. And (3) testing conditions are as follows: c 18 A chromatographic column: 250 × 4.6mm, column temperature: 30 degrees; sample introduction amount: 20 ul; wavelength: 254 nm; methanol: 0.2% phosphoric acid water isocratic elution 45: 55; flow rate: 1 ml/min.
On the other hand, 29 characteristic flavor substances in the fresh kernel are measured by adopting gas phase ion mobility chromatography, namely: weighing 3.00g of crushed fresh nucleolus sample, placing the crushed fresh nucleolus sample into a 20mL headspace sample injection bottle for incubation, extracting headspace components in the bottle by using a heated sample injection needle, and analyzing volatile components by using a Flavour Spec gas phase ion mobility spectrometer. Specifically, the GC-IMS measurement conditions were: the headspace incubation temperature is 50 ℃, the incubation time is 10min, and the incubation rotation speed is 500 r/min. The carrier gas is high-purity nitrogen (not less than 99.999%), the temperature of the chromatographic column is 40 ℃, the chromatographic operation time is 20min, the flow rate gradient of the carrier gas is set to be 2.00mL/min and is kept for 2min, the flow rate gradient is linearly increased to 20.00mL/min within 6min, and the flow rate gradient is linearly increased to 100.00mL/min within 2min and is kept for 5 min. The headspace sampling needle temperature is 55 ℃, the sampling amount is 500 mu L, the non-shunting mode is adopted, and the cleaning time is 0.50 min. And (3) data analysis: analyzing the spectrum by using LAV (laboratory Analytical viewer) software, and constructing a difference map and a fingerprint map of the volatile organic compounds by using a Reporter and a Gallery plug-in program; the software is internally provided with an NIST database and an IMS database to carry out qualitative analysis on substances, and requires that fresh walnut kernels must contain propionaldehyde, isopropanol (monomer), isopropanol (dimer), trans-2, 4-heptadienal, isoamyl acetate (monomer), isoamyl acetate (dimer), propyl acetate, 2-methylbutanol (monomer), 2-methylbutanol (dimer), isobutyl acetate, ethyl 3-hydroxybutyrate (monomer), ethyl 3-hydroxybutyrate (dimer), 3-hydroxy-2-butanone (monomer), 3-hydroxy-2-butanone (dimer), ethyl acrylate, acetic acid (monomer), acetic acid (dimer), isopropyl acetate (monomer), isopropyl acetate (dimer), 2-methylbutanal, n-butanal, isopropyl acetate (dimer), 2-methylbutanal, n-butanal, and n-butanal, 2-butanone (monomer), 2-butanone (dimer), 2-methylacrolein, n-hexanal, 3-pentanone, 2-hexanone, 3-hydroxy-2-butanone and 3-methyl-2-butenal, and 29 characteristic flavor substances. Only when the arbutin content in the green tangerine peel and the characteristic components of the kernel both meet the requirements, the walnut is Xinjiang 'warm 185' thin-skinned fresh walnut.
The foregoing description of specific embodiments of the present invention has been presented. It is to be understood that the present invention is not limited to the specific embodiments described above, and that various changes and modifications may be made by one skilled in the art within the scope of the appended claims without departing from the spirit of the invention.
Claims (3)
1. A method for identifying Xinjiang 'warm 185' thin-skinned fresh walnuts is characterized by comprising the following steps: the method comprises the following steps:
s1, measuring the arbutin content in the 'warm 185' thin-skinned walnut green peel by adopting a liquid chromatography, wherein the arbutin content is required to reach 100-150 mug/g;
s2, determining characteristic flavor substances in fresh kernel by gas phase ion mobility chromatography, wherein fresh walnut kernel is required to contain propionaldehyde, isopropanol (monomer), isopropanol (dimer), trans-2, 4-heptadienal, isoamyl acetate (monomer), isoamyl acetate (dimer), propyl acetate, 2-methylbutanol (monomer), 2-methylbutanol (dimer), isobutyl acetate, ethyl 3-hydroxybutyrate (monomer), ethyl 3-hydroxybutyrate (dimer), 3-hydroxy-2-butanone (monomer), 3-hydroxy-2-butanone (dimer), ethyl acrylate, acetic acid (monomer), acetic acid (dimer), isopropyl acetate (monomer), isopropyl acetate (dimer), 2-methylbutanal, and isopropyl acetate (monomer), N-butyraldehyde, 2-butanone (monomer), 2-butanone (dimer), 2-methylacrolein, n-hexanal, 3-pentanone, 2-hexanone, 3-hydroxy-2-butanone, 3-methyl-2-butenal.
2. The method for identifying Xinjiang 'warm 185' thin-skinned fresh walnuts as claimed in claim 1, wherein: step S1 specifically includes the following steps:
accurately weighing 3g of fresh walnut jelly, adding 80% methanol water into a 15ml brown centrifuge tube according to the material-liquid ratio of 1:10, shaking and mixing for 5min, and performing ultrasonic extraction for 30miAfter n, centrifuging for 15min at 4000 r/min; transferring the supernatant into another centrifuge tube, repeatedly extracting for 2 times, mixing the supernatants for 3 times, reducing the pressure of nitrogen at room temperature to dryness, dissolving with 20% acetonitrile water to constant volume of 10ml, shaking, mixing, and filtering with 0.45 μm filter membrane to be detected; and (3) testing conditions are as follows: c 18 A chromatographic column: 250 × 4.6mm, column temperature: 30 degrees; sample introduction amount: 20 ul; wavelength: 254 nm; methanol: 0.2% phosphoric acid water isocratic elution 45: 55; flow rate: 1 ml/min.
3. The method for identifying Xinjiang 'Wen 185' thin-skinned fresh walnuts as claimed in claim 1, wherein: step S2 specifically includes the following steps:
weighing 3.00g of crushed fresh nucleolus sample, placing the crushed fresh nucleolus sample into a 20mL headspace sample injection bottle for incubation, extracting headspace components in the bottle by using a heated sample injection needle, and analyzing volatile components by using a Flavour Spec gas phase ion mobility spectrometer; wherein, the GC-IMS determination conditions are as follows: the headspace incubation temperature is 50 ℃, the incubation time is 10min, and the incubation rotation speed is 500 r/min; the carrier gas is high-purity nitrogen (not less than 99.999%), the temperature of the chromatographic column is 40 ℃, the chromatographic operation time is 20min, the flow rate gradient of the carrier gas is set to be 2.00mL/min and kept for 2min, the flow rate gradient is linearly increased to 20.00mL/min within 6min, and the flow rate gradient is linearly increased to 100.00mL/min within 2min and kept for 5 min; the headspace sampling needle temperature is 55 ℃, the sampling amount is 500 mu L, a non-shunting mode is adopted, and the cleaning time is 0.50 min; and (3) data analysis: analyzing the spectrum by adopting LAV (laboratory Analytical viewer) software, and constructing a difference map and a fingerprint map of the volatile organic compounds by adopting a Reporter and a Gallery plug-in program; the software is internally provided with an NIST database and an IMS database to carry out qualitative analysis on the substances.
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| CN110836934A (en) * | 2019-11-22 | 2020-02-25 | 成都中医药大学 | Construction method and identification application of peach kernel and walnut kernel analytical model |
| CN113109486A (en) * | 2021-05-14 | 2021-07-13 | 新疆林业科学院 | Method for identifying walnut seeds based on GC-IMS analysis leaves |
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| Publication number | Priority date | Publication date | Assignee | Title |
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