CN108802222B - Method for identifying winter honey and Chinese tallow tree honey based on volatile substances - Google Patents

Method for identifying winter honey and Chinese tallow tree honey based on volatile substances Download PDF

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CN108802222B
CN108802222B CN201810607157.9A CN201810607157A CN108802222B CN 108802222 B CN108802222 B CN 108802222B CN 201810607157 A CN201810607157 A CN 201810607157A CN 108802222 B CN108802222 B CN 108802222B
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honey
detected
tallow tree
chinese tallow
response value
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CN108802222A (en
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周金慧
李熠
王欣然
杨术鹏
张金振
金玥
赵文
黄京平
王鹏
袁媛
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Institute of Apicultural Research of Chinese Academy of Agricultural Sciences
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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
    • 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
    • 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
    • G01N30/14—Preparation by elimination of some components
    • 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
    • G01N30/62—Detectors specially adapted therefor
    • G01N30/72—Mass spectrometers
    • 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
    • G01N30/86—Signal analysis
    • G01N30/8696—Details of Software

Abstract

The invention relates to the field of testing, and particularly relates to a method for identifying winter honey and Chinese tallow tree honey based on volatile substances. The identification method provided by the invention is characterized in that one or two or three of furanone dimer, 2-octanone or hexanol dimer are used as markers. The method does not need a sample pretreatment process, is simple and quick to operate, is environment-friendly, and has completely visualized characteristic regions. In conclusion, the invention provides a simple and quick identification method, which is of great significance for quickly identifying winter honey, Chinese tallow tree honey and adulterated honey mixed with the Chinese tallow tree honey in the winter honey, promoting the industrialized development of bee products and being beneficial to the health and sustainable development of the bee-keeping industry.

Description

Method for identifying winter honey and Chinese tallow tree honey based on volatile substances
Technical Field
The invention relates to the field of testing, and particularly relates to a method for identifying winter honey and Chinese tallow tree honey based on volatile substances.
Background
The honey is natural sweet substance obtained by collecting nectar, secretion or honeydew of plants by bees, combining with secretion, and brewing. Differences in bee species, honey source plants and production places can all result in differences in endogenous active components in honey.
The winter honey is usually honey collected by Chinese bees in winter, mainly comes from honey source plants such as schefflera octophylla and wild osmanthus fragrans, is a specific honey species in the south of the Ling, and is called winter honey. The concentration of honey is higher than that of honey harvested in other seasons due to dry climate in winter, and the honey is amber, easy to crystallize and fine in texture, so winter honey is called as high-quality honey in the beekeeping industry. The winter honey has the efficacies of clearing heat, tonifying middle-jiao, detoxifying, moistening dryness and the like of most honey, also has the efficacies of inducing sweat, relieving exterior syndrome, dispelling wind and eliminating dampness, and has better auxiliary curative effects on cold, fever, sore throat and rheumatic arthralgia.
The Chinese tallow tree honey is brewed by collecting Chinese tallow tree flower honey by bees, is amber, has slight fermentation acid smell, has poor throat moistening feeling, is easy to crystallize and coarse, so consumers do not like to directly eat the honey.
The taste difference of winter honey and Chinese tallow tree honey causes different preference of consumers to the two kinds of honey, so that the price of the two kinds of honey is obviously different, lawless persons use the Chinese tallow tree honey to be overflowed or mixed into the winter honey to be insufficient for pursuing high profit, serious economic loss is caused to vast Chinese bee farmers and related enterprises in China, and the healthy development of the Chinese bee industry is restricted.
Disclosure of Invention
Until now, no research method for identifying winter honey and Chinese tallow tree honey exists. Therefore, it is necessary to establish a simple, rapid and accurate chemical analysis method and find a characteristic marker for identifying the two types of honey. In recent years, the advantages of simple operation of gas chromatography-ion mobility spectrometry, no need of sample pretreatment, environmental friendliness, short analysis time and the like play an important role in the identification of edible oil and Chinese herbal medicines, but no relevant report is found in the identification research aspect of honey varieties.
The invention relates to a method for identifying winter honey and Chinese tallow tree honey, which is realized by selecting a specific marker.
Specifically, the invention is realized by the following technical scheme:
the method of the invention is characterized in that one or two or three of furanone dimer, 2-octanone or hexanol dimer is used as a marker for identification.
Namely, the method for identifying winter honey and Chinese tallow tree honey takes furanone dimer as a marker; or 2-octanone is taken as a marker; or, hexanol dimer as a marker; or, furanone dimer and 2-octanone are used as markers; or, furanone dimer and hexanol dimer as markers; or, 2-octanone and hexanol dimer as markers; or three of furanone dimer, 2-octanone and hexanol dimer are used as markers.
Preferably, the method adopts gas chromatography-ion mobility spectrometry to identify by using the difference of the response values of the markers;
the invention firstly finds that the gas chromatography-ion mobility spectrometry is combined, and the difference of response values is used for identifying the winter honey and the Chinese tallow tree honey.
Preferably, the method further comprises incubating the honey to be tested before sample injection, wherein the incubation time is 20-30min, and the incubation temperature is 55-65 ℃; preferably the incubation temperature is 55 ℃. Preferably, the mass of the honey to be detected is 2-5 g.
By adopting the hatching mode of the products to be tested, partial components in the honey can be volatilized, the components can not be damaged, and the accuracy of results can not be influenced.
Preferably, the furanone dimer is used as a marker, when the response value is 57-192mv, the honey to be detected is winter honey, and when the response value is not in the range, the honey to be detected is mixed honey or Chinese tallow tree honey; when the response value is 11-16mv, the honey to be detected is Chinese tallow tree honey;
taking 2-octanone as a marker, when the response value is 98-250mv, the honey to be detected is winter honey, and when the response value is not in the range, the honey to be detected is mixed honey or Chinese tallow tree honey; when the response value is 12-27mv, the honey to be detected is Chinese tallow tree honey;
taking hexanol dimer as a marker, when the response value is 10-17mv, the honey to be detected is winter honey, and when the response value is not in the range, the honey to be detected is mixed honey or Chinese tallow tree honey; when the response value is 27-55mv, the honey to be detected is Chinese tallow tree honey;
further, in the actual detection environment, the adulteration concentration is not lower than 5%, but higher than 50% can be clearly identified through senses, and in the actual application, the main adulteration range is 5% -50%, so the response value of the adulteration range is provided by the invention.
Taking furanone dimer as a marker, wherein the response value is 26-40mv, and the honey to be detected is mixed honey of winter honey and Chinese tallow tree honey;
taking 2-octanone as a marker, wherein the response value is 18-72mv, and the honey to be detected is mixed honey of winter honey and Chinese tallow tree honey;
and taking hexanol dimer as a marker, wherein the response value is 20-48mv, and the honey to be detected is mixed honey of winter honey and Chinese tallow tree honey.
Preferably, in the method of the present invention, the gas chromatography uses a weak-polarity capillary chromatography column; and then, according to the response value of the marker in the spectrogram of the to-be-detected product, identification can be carried out.
Preferably, the IMS temperature is controlled to be 40-50 ℃ during the ion migration.
Specifically, the authentication method of the present invention comprises the steps of:
1) taking honey to be detected, and allowing the honey to enter a gas chromatography-ion mobility spectrometer to obtain a spectrogram of a product to be detected;
wherein the content of the first and second substances,
the chromatographic column conditions were: column temperature: 55-65 deg.C (preferably 60 deg.C); carrier gas flow: 0-2min,2mL/min, 2-20min,2mL/min-100 mL/min; drift gas flow rate: 150 mL/min; carrier gas/drift gas: n is a radical of2；
And/or, the ion mobility spectrometry conditions are: temperature of the sample injection needle: 80-85 ℃; sample introduction volume: 450-;
2) and identifying according to the response value of the marker in the spectrogram of the to-be-detected product.
In the step 1), preferably, the chromatographic column is SE-54; more preferably FS-SE-54-CB-0.5(15m, ID:0.53 mm).
Specifically, the SE-54 column is a (5% -phenyl) (1% -vinyl) -methylpolysiloxane chromatography column. Conventional non-bonded columns based on poly (4% methyl/5% phenyl) siloxane; this phase also contained 1% vinyl groups. The material of the column is Fused Silica (FS).
The chromatographic column conditions were: carrier gas flow: 0-2min,2mL/min, 2-20min,2mL/min-100 mL/min; drift gas flow rate: 150 mL/min; carrier gas/drift gas: n is a radical of2；
Preferably, the ion mobility spectrometry conditions are: IMS temperature: 45 ℃; temperature of the sample injection needle: 85 ℃; sample introduction volume: 500 μ L.
The invention determines the marker by the following method:
background subtraction, chromatographic peak extraction and peak alignment of data of two groups of honey samples of winter honey and Chinese tallow tree honey are performed by using a gas chromatography-ion mobility spectrometer with LAV (laboratory Analytical viewer) software. And searching the obtained ion current spectrum data in an NIST library, finally identifying endogenous component information in the two types of honey, and obtaining characteristic markers capable of identifying the two types of honey through screening and experiments. Correspondingly, the honey to be tested is treated in the same way.
The invention firstly applies the gas chromatography-ion mobility spectrometry analysis technology to the analysis of winter honey and Chinese tallow tree honey samples, and meanwhile, the honey to-be-detected product does not need any pretreatment, thereby not only reducing the operation difficulty and saving the cost, but also further avoiding the interference of external solvents and greatly increasing the detection accuracy. The instrument conditions are properly controlled, so that volatile substances in the honey can be volatilized as far as possible, and the phenomenon that the volatile substance structure is dissociated to cause the loss of useful information due to excessive conditions is avoided. The method is simple and rapid to operate, environment-friendly and completely visualized in the characteristic region.
In conclusion, the invention provides a simple and rapid gas chromatography-ion mobility spectrometry analysis method, which has important significance for rapidly identifying winter honey, Chinese tallow tree honey and adulterated honey mixed with the winter honey, promoting the industrialized development of bee products and being beneficial to the health and sustainable development of the bee-keeping industry.
Drawings
FIG. 1 is a box diagram showing the difference in response values between Furanone dimer (Furanone dimer) and 2-Octanone (2-Octanone) which are characteristic markers of winter honey, Chinese tallow tree honey and adulterated honey according to the present invention, wherein the abscissa is the response value and the ordinate is the sample; (D: Chinese tallow tree honey; W: Chinese tallow tree honey; C: adulterated honey which is prepared by respectively adding 5% of Chinese tallow tree honey, 10% of Chinese tallow tree honey, 20% of Chinese tallow tree honey, 30% of Chinese tallow tree honey, 40% of Chinese tallow tree honey and 50% of Chinese tallow tree honey into Chinese tallow tree honey);
FIG. 2 is a box diagram showing the difference in response values of Hexanol dimer (1-Hexanol dimer) which is a characteristic marker in winter honey, Chinese tallow tree honey and adulterated honey according to the present invention, wherein the abscissa is the response value and the ordinate is the sample; (D: Chinese tallow tree honey; W: Chinese tallow tree honey; C: adulterated honey which is prepared by respectively adding 5% of Chinese tallow tree honey, 10% of Chinese tallow tree honey, 20% of Chinese tallow tree honey, 30% of Chinese tallow tree honey, 40% of Chinese tallow tree honey and 50% of Chinese tallow tree honey) into Chinese tallow tree honey.
Detailed Description
The following examples are intended to illustrate the invention but are not intended to limit the scope of the invention.
Example 1
The embodiment provides a method for identifying winter honey and Chinese tallow tree honey, which takes furanone dimer as a marker and specifically comprises the following steps:
1) the pretreatment method of the honey sample comprises the following steps: weighing 2.0 +/-0.1 g of honey to be tested in each part, placing the honey in a 20mL headspace sample injection bottle, and incubating for: 20 min; incubation temperature: 55 ℃; after incubation, separation was performed on a gas chromatography-ion mobility spectrometer.
The instrument conditions were: a chromatographic column: FS-SE-54-CB-0.5(15m, ID:0.53 mm); column temperature: 60 ℃; carrier gas flow: 0-2min,2mL/min, 2-20min,2mL/min-100 mL/min; drift gas flow rate: 150 mL/min; carrier gas/drift gas: n is a radical of2(ii) a IMS temperature: 45 ℃; temperature of the sample injection needle: 85 ℃; sample introduction volume: 500 μ L.
2) And (3) data analysis:
carrying out background subtraction, chromatographic peak extraction and peak alignment on the spectrogram obtained in the step 1), and then carrying out maximum value normalization processing on the spectrogram to be used as a judgment basis; then, judging according to the response value of the characteristic marker furanone dimer: the response value range of furanone dimer in winter honey is 57-192mv, and the content range of Chinese tallow tree honey is 11-16mv, and the furanone dimer content range in the sample mixed with Chinese tallow tree honey is 26-40 mv.
Example 2
The embodiment provides a method for identifying winter honey and Chinese tallow tree honey, which takes 2-octanone as a marker and specifically comprises the following operations:
1) the pretreatment method of the honey sample comprises the following steps: weighing 2.0 +/-0.1 g of honey in each part, placing the honey in a 20mL headspace sample injection bottle, and incubating for: 20 min; incubation temperature: 55 ℃; after incubation, separation was performed on a gas chromatography-ion mobility spectrometer.
The instrument conditions were: a chromatographic column: FS-SE-54-CB-0.5(15m, ID:0.53 mm); column temperature: 60 ℃; carrier gas flow: 0-2min,2mL/min, 2-20min,2mL/min-100 mL/min; drift gas flow rate: 150 mL/min; carrierGas/drift gas: n is a radical of2(ii) a IMS temperature: 45 ℃; temperature of the sample injection needle: 85 ℃; sample introduction volume: 500 μ L.
2) And (3) data analysis:
carrying out background subtraction, chromatographic peak extraction and peak alignment on the spectrogram obtained in the step 1), and then carrying out maximum value normalization processing on the spectrogram to be used as a judgment basis; then, judging according to the response value of the characteristic marker 2-octanone: the response value range of 2-octanone in winter honey is 98-250mv, and the content range of 2-octanone in Chinese tallow tree honey is 12-27mv, and the 2-octanone content in the sample mixed with winter honey is 18-72 mv.
Example 3
The embodiment provides a method for identifying winter honey and Chinese tallow tree honey, which takes hexanol dimer as a marker and specifically comprises the following steps:
1) the pretreatment method of the honey sample comprises the following steps: weighing 2.0 +/-0.1 g of honey in each part, placing the honey in a 20mL headspace sample injection bottle, and incubating for: 20 min; incubation temperature: 55 ℃; after incubation, separation was performed on a gas chromatography-ion mobility spectrometer.
The instrument conditions were: a chromatographic column: FS-SE-54-CB-0.5(15m, ID:0.53 mm); column temperature: 60 ℃; carrier gas flow: 0-2min,2mL/min, 2-20min,2mL/min-100 mL/min; drift gas flow rate: 150 mL/min; carrier gas/drift gas: n is a radical of2(ii) a IMS temperature: 45 ℃; temperature of the sample injection needle: 85 ℃; sample introduction volume: 500 μ L.
2) And (3) data analysis:
carrying out background subtraction, chromatographic peak extraction and peak alignment on the spectrogram obtained in the step 1), and then carrying out maximum value normalization processing on the spectrogram to be used as a judgment basis; then judging according to the response value of the characteristic marker hexanol dimer: the hexanol dimer response value in winter honey is 10-17mv, while the sapium sebiferum honey is 27-55mv, and the hexanol dimer content in the sample mixed with the winter honey is 20-48 mv.
Example 4
The embodiment provides a method for identifying winter honey and Chinese tallow tree honey, which takes furanone dimer and 2-octanone as markers and specifically comprises the following steps:
1) the pretreatment method of the honey sample comprises the following steps: weighing 2.0 +/-0.1 g of honey in each part, placing the honey in a 20mL headspace sample injection bottle, and incubating for: 20 min; incubation temperature: 55 ℃; after incubation, separation was performed on a gas chromatography-ion mobility spectrometer.
The instrument conditions were: a chromatographic column: FS-SE-54-CB-0.5(15m, ID:0.53 mm); column temperature: 60 ℃; carrier gas flow: 0-2min,2mL/min, 2-20min,2mL/min-100 mL/min; drift gas flow rate: 150 mL/min; carrier gas/drift gas: n is a radical of2(ii) a IMS temperature: 45 ℃; temperature of the sample injection needle: 85 ℃; sample introduction volume: 500 μ L.
2) And (3) data analysis:
carrying out background subtraction, chromatographic peak extraction and peak alignment on the spectrogram obtained in the step 1), and then carrying out maximum value normalization processing on the spectrogram to be used as a judgment basis; then, judging according to the response values of characteristic markers of furanone dimer and 2-octanone:
characteristic marker furanone dimer: the response value range of furanone dimer in winter honey is 57-192mv, and the content range of Chinese tallow tree honey is 11-16mv, and the furanone dimer content range in the sample mixed with Chinese tallow tree honey is 26-40 mv.
Characteristic marker 2-octanone: the response value range of 2-octanone in winter honey is 98-250mv, and the content range of 2-octanone in Chinese tallow tree honey is 12-27mv, and the 2-octanone content in the sample mixed with winter honey is 18-72 mv.
Example 5
This example provides a method for identifying winter honey and Chinese tallow tree honey, which uses furanone dimer and hexanol dimer as markers, and specifically comprises the following steps:
1) the pretreatment method of the honey sample comprises the following steps: weighing 2.0 +/-0.1 g of honey in each part, placing the honey in a 20mL headspace sample injection bottle, and incubating for: 20 min; incubation temperature: 55 ℃; after incubation, separation was performed on a gas chromatography-ion mobility spectrometer.
The instrument conditions were: a chromatographic column: FS-SE-54-CB-0.5(15m, ID:0.53 mm); column temperature: 60 ℃; carrier gas flow: 0-2min,2mL/min, 2-20min,2mL/min-100 mL/min; drift gas flow rate: 150 mL/min; carrier gas/drift gas: n is a radical of2(ii) a IMS temperature: 45 ℃; temperature of the sample injection needle: 85 ℃; sample introduction volume: 500 μ L.
2) And (3) data analysis:
carrying out background subtraction, chromatographic peak extraction and peak alignment on the spectrogram obtained in the step 1), and then carrying out maximum value normalization processing on the spectrogram to be used as a judgment basis; then, the judgment is carried out according to the response values of the characteristic markers of furanone dimer and hexanol dimer:
characteristic marker furanone dimer: the response value range of furanone dimer in winter honey is 57-192mv, and the content range of Chinese tallow tree honey is 11-16mv, and the furanone dimer content range in the sample mixed with Chinese tallow tree honey is 26-40 mv.
Characteristic markers hexanol dimer: the hexanol dimer response value in winter honey is 10-17mv, while the sapium sebiferum honey is 27-55mv, and the hexanol dimer content in the sample mixed with the winter honey is 20-48 mv.
Example 6
This example provides a method for identifying winter honey and Chinese tallow tree honey, which uses furanone dimer, 2-octanone and hexanol dimer as markers, and specifically comprises the following steps:
1) the pretreatment method of the honey sample comprises the following steps: weighing 2.0 +/-0.1 g of honey in each part, placing the honey in a 20mL headspace sample injection bottle, and incubating for: 20 min; incubation temperature: 55 ℃; after incubation, separation was performed on a gas chromatography-ion mobility spectrometer.
The instrument conditions were: a chromatographic column: FS-SE-54-CB-0.5(15m, ID:0.53 mm); column temperature: 60 ℃; carrier gas flow: 0-2min,2mL/min, 2-20min,2mL/min-100 mL/min; drift gas flow rate: 150 mL/min; carrier gas/drift gas: n is a radical of2(ii) a IMS temperature: 45 ℃; temperature of the sample injection needle: 85 ℃; sample introduction volume: 500 μ L.
2) And (3) data analysis:
carrying out background subtraction, chromatographic peak extraction and peak alignment on the spectrogram obtained in the step 1), and then carrying out maximum value normalization processing on the spectrogram to be used as a judgment basis; then, the judgment is carried out according to the response values of characteristic markers of furanone dimer, 2-octanone and hexanol dimer:
characteristic marker furanone dimer: the response value range of furanone dimer in winter honey is 57-192mv, and the content range of Chinese tallow tree honey is 11-16mv, and the furanone dimer content range in the sample mixed with Chinese tallow tree honey is 26-40 mv.
Characteristic marker 2-octanone: the response value range of 2-octanone in winter honey is 98-250mv, and the content range of 2-octanone in Chinese tallow tree honey is 12-27mv, and the 2-octanone content in the sample mixed with winter honey is 18-72 mv.
Characteristic markers hexanol dimer: the hexanol dimer response value in winter honey is 10-17mv, while the sapium sebiferum honey is 27-55mv, and the hexanol dimer content in the sample mixed with the winter honey is 20-48 mv.
Example 7
The embodiment provides a method for identifying winter honey and Chinese tallow tree honey, which specifically comprises the following operations:
1) the pretreatment method of the honey sample comprises the following steps: weighing 2.0 +/-0.1 g of honey in each part, placing the honey in a 20mL headspace sample injection bottle, and incubating for: 20 min; incubation temperature: 55 ℃; the separation was performed on a gas chromatography-ion mobility spectrometer.
The instrument conditions were: a chromatographic column: FS-SE-54-CB-0.5(15m, ID:0.53 mm); column temperature: 60 ℃; carrier gas flow: 0-2min,2mL/min, 2-20min,2mL/min-100 mL/min; drift gas flow rate: 150 mL/min; carrier gas/drift gas: n is a radical of2(ii) a IMS temperature: 45 ℃; temperature of the sample injection needle: 85 ℃; sample introduction volume: 500 mu L of the solution; incubation time: 20 min; incubation temperature: at 55 ℃.
2) And (3) data analysis:
carrying out background subtraction, chromatographic peak extraction and peak alignment on the spectrogram obtained in the step 1), and then carrying out maximum value normalization processing on the spectrogram to be used as a judgment basis; then, the furanone dimer is taken as a characteristic marker, and the response value is 26-40 mv; and judging that the honey to be detected is mixed honey of winter honey and Chinese tallow tree honey.
Example 8
The embodiment provides a method for identifying winter honey and Chinese tallow tree honey, which specifically comprises the following operations:
1) the pretreatment method of the honey sample comprises the following steps: weighing 2.0 +/-0.1 g of honey in each part, placing the honey in a 20mL headspace sample injection bottle, and incubating for: 20 min; incubation temperature: 55 ℃; the separation was performed on a gas chromatography-ion mobility spectrometer.
The instrument conditions were: a chromatographic column: FS-SE-54-CB-0.5(15m, ID:0.53 mm); column temperature: 60 ℃; carrier gas flow: 0-2min,2mL/min, 2-20min,2mL/min-100 mL/min; drift gas flow rate: 150 mL/min; carrier gas/drift gas: n is a radical of2(ii) a IMS temperature: 45 ℃; temperature of the sample injection needle: 85 ℃; sample introduction volume: 500 mu L of the solution; incubation time: 20 min; incubation temperature: at 55 ℃.
2) And (3) data analysis:
carrying out background subtraction, chromatographic peak extraction and peak alignment on the spectrogram obtained in the step 1), and then carrying out maximum value normalization processing on the spectrogram to be used as a judgment basis; then 2-octanone is taken as a marker, and the response value is 18-72 mv; and judging that the honey to be detected is mixed honey of winter honey and Chinese tallow tree honey.
Example 9
The embodiment provides a method for identifying winter honey and Chinese tallow tree honey, which specifically comprises the following operations:
1) the pretreatment method of the honey sample comprises the following steps: weighing 2.0 +/-0.1 g of honey in each part, placing the honey in a 20mL headspace sample injection bottle, and incubating for: 20 min; incubation temperature: 55 ℃; the separation was performed on a gas chromatography-ion mobility spectrometer.
The instrument conditions were: a chromatographic column: FS-SE-54-CB-0.5(15m, ID:0.53 mm); column temperature: 60 ℃; carrier gas flow: 0-2min,2mL/min, 2-20min,2mL/min-100 mL/min; drift gas flow rate: 150 mL/min; carrier gas/drift gas: n is a radical of2(ii) a IMS temperature: 45 ℃; temperature of the sample injection needle: 85 ℃; sample introduction volume: 500 mu L of the solution; incubation time: 20 min; incubation temperature: at 55 ℃.
2) And (3) data analysis:
carrying out background subtraction, chromatographic peak extraction and peak alignment on the spectrogram obtained in the step 1), and then carrying out maximum value normalization processing on the spectrogram to be used as a judgment basis; and then judging that the honey to be detected is mixed honey of winter honey and Chinese tallow tree honey by taking hexanol dimer as a marker and the response value of 20-48 mv.
Test example 1
The test example provides accuracy verification of the method for identifying winter honey and Chinese tallow tree honey, and the method specifically comprises the following operations:
1) preparing a honey sample: mixed honey of 5 wt% of Chinese tallow tree honey is doped in winter honey;
2) the pretreatment method of the honey sample comprises the following steps: weighing 3.5 +/-0.1 g of the mixed honey in each part, placing the mixed honey into a 20mL headspace sample injection bottle, and incubating for: 20 min; incubation temperature: 55 ℃; the separation was performed on a gas chromatography-ion mobility spectrometer.
The instrument conditions were: a chromatographic column: FS-SE-54-CB-0.5(15m, ID:0.53 mm); column temperature: 60 ℃; carrier gas flow: 0-2min,2mL/min, 2-20min,2mL/min-100 mL/min; drift gas flow rate: 150 mL/min; carrier gas/drift gas: n is a radical of2(ii) a IMS temperature: 45 ℃; temperature of the sample injection needle: 85 ℃; sample introduction volume: 500 μ L.
3) And (3) data analysis:
carrying out background subtraction, chromatographic peak extraction and peak alignment on the spectrogram obtained in the step 1), and then carrying out maximum value normalization processing on the spectrogram to be used as a judgment basis;
the data obtained were: the response value of the characteristic marker furanone dimer is 26 mv;
the response value of furanone dimer in the sample doped with Chinese tallow tree honey is 26-40mv, and the honey adopted in the test example is mixed honey.
According to the test example, even if the mixing amount of the Chinese tallow tree honey is as low as 5 wt%, the detection can be realized according to the method provided by the invention.
Test example 2
The test example provides accuracy verification of the method for identifying winter honey and Chinese tallow tree honey, and the method specifically comprises the following operations:
1) preparing a honey sample: mixed honey of 5 wt% of Chinese tallow tree honey is doped in winter honey;
2) the pretreatment method of the honey sample comprises the following steps: weighing 3.5 +/-0.1 g of the mixed honey in each part, placing the mixed honey into a 20mL headspace sample injection bottle, and incubating for: 20 min; incubation temperature: 55 ℃; the separation was performed on a gas chromatography-ion mobility spectrometer.
The instrument conditions were: a chromatographic column: FS-SE-54-CB-0.5(15m, ID:0.53 mm); column temperature: 60 ℃; carrier gas flow: 0-2min,2mL/min, 2-20min,2mL/min-100 mL/min; drift gas flow rate: 150 mL/min; carrier gas/drift gas: n is a radical of2(ii) a IMS temperature: 45 ℃; temperature of the sample injection needle: 85 ℃; sample introduction volume: 500 μ L.
3) And (3) data analysis:
carrying out background subtraction, chromatographic peak extraction and peak alignment on the spectrogram obtained in the step 1), and then carrying out maximum value normalization processing on the spectrogram to be used as a judgment basis; the resulting data were then: the response value of the characteristic marker 2-octanone is 18 mv;
according to the judgment that the response value is 18-72mv when 2-octanone is taken as a marker, the honey to be tested is mixed honey of winter honey and Chinese tallow tree honey, and the honey adopted in the test example is mixed honey.
According to the test example, even if the mixing amount of the Chinese tallow tree honey is as low as 5 wt%, the detection can be realized according to the method provided by the invention.
Test example 3
The test example provides accuracy verification of the method for identifying winter honey and Chinese tallow tree honey, and the method specifically comprises the following operations:
1) preparing a honey sample: mixed honey of 5 wt% of Chinese tallow tree honey is doped in winter honey;
2) the pretreatment method of the honey sample comprises the following steps: weighing 3.5 +/-0.1 g of the mixed honey in each part, placing the mixed honey into a 20mL headspace sample injection bottle, and incubating for: 20 min; incubation temperature: 55 ℃; the separation was performed on a gas chromatography-ion mobility spectrometer.
The instrument conditions were: a chromatographic column: FS-SE-54-CB-0.5(15m, ID:0.53 mm); column temperature: 60 ℃; carrier gas flow: 0-2min,2mL/min, 2-20min,2mL/min-100 mL/min; drift gas flow rate: 150 mL/min; carrier gas/drift gas: n is a radical of2(ii) a IMS temperature: 45 ℃; temperature of the sample injection needle: 85 ℃; sample introduction volume: 500 μ L.
3) And (3) data analysis:
carrying out background subtraction, chromatographic peak extraction and peak alignment on the spectrogram obtained in the step 1), and then carrying out maximum value normalization processing on the spectrogram to be used as a judgment basis; the resulting data were then: the response value of the characteristic marker hexanol dimer is 20 mv;
according to the fact that hexanol dimer is used as a marker, the response value is 20-48mv, the honey to be detected is mixed honey of winter honey and Chinese tallow tree honey, and the honey adopted in the test example is the mixed honey.
According to the test example, even if the mixing amount of the Chinese tallow tree honey is as low as 5 wt%, the detection can be realized according to the method provided by the invention.
Test example 4
The embodiment provides a method for identifying winter honey and Chinese tallow tree honey, which specifically comprises the following operations:
1) preparing a honey sample: respectively preparing mixed honey of 10 wt%, 20 wt%, 30 wt%, 40 wt% and 50 wt% of Chinese tallow tree honey in winter honey;
2) the pretreatment method of the honey sample comprises the following steps: weighing 3.5 +/-0.1 g of the mixed honey in each part, placing the mixed honey into a 20mL headspace sample bottle, and incubating for: 20 min; incubation temperature: 55 ℃; and then the separation is carried out on a gas chromatography-ion mobility spectrometer respectively.
The instrument conditions were: a chromatographic column: FS-SE-54-CB-0.5(15m, ID:0.53 mm); column temperature: 60 ℃; carrier gas flow: 0-2min,2mL/min, 2-20min,2mL/min-100 mL/min; drift gas flow rate: 150 mL/min; carrier gas/drift gas: n is a radical of2(ii) a IMS temperature: 45 ℃; temperature of the sample injection needle: 85 ℃; sample introduction volume: 500 μ L.
3) And (3) data analysis:
carrying out background subtraction, chromatographic peak extraction and peak alignment on the spectrogram obtained in the step 1), and then carrying out maximum value normalization processing on the spectrogram to be used as a judgment basis; the data obtained are then shown in the following table:
TABLE 1 response value data for mixed honey samples
Figure GDA0003115772960000141
According to the response values of the characteristic markers, the results of the identification method provided by the test example are accurate.
Although the invention has been described in detail hereinabove by way of general description, specific embodiments and experiments, it will be apparent to those skilled in the art that many modifications and improvements can be made thereto based on the invention. Accordingly, such modifications and improvements are intended to be within the scope of the invention as claimed.

Claims (6)

1. A method for identifying winter honey and Chinese tallow tree honey based on volatile substances is characterized in that a gas chromatography-ion mobility spectrometry analysis method is adopted, and response value differences of markers are used for identification; wherein, furanone dimer, 2-octanone and hexanol dimer are used as markers; or, furanone dimer and 2-octanone are used as markers; or, furanone dimer and hexanol dimer as markers;
taking furanone dimer as a marker, when the response value is 57-192mv, the honey to be detected is winter honey, and when the response value is not in the range, the honey to be detected is mixed honey or Chinese tallow tree honey; when the response value is 11-16mv, the honey to be detected is Chinese tallow tree honey;
taking 2-octanone as a marker, taking honey to be detected as winter honey when the response value is 98-250mv, and taking honey to be detected as mixed honey or Chinese tallow tree honey when the response value is not in the range; when the response value is 12-27mv, the honey to be detected is Chinese tallow tree honey;
taking hexanol dimer as a marker, when the response value is 10-17mv, the honey to be detected is winter honey, and when the response value is not in the range, the honey to be detected is mixed honey or Chinese tallow tree honey; when the response value is 27-55mv, the honey to be detected is Chinese tallow tree honey;
the method specifically comprises the following steps:
1) taking honey to be detected, and allowing the honey to enter a gas chromatography-ion mobility spectrometer to obtain a spectrogram of a product to be detected;
wherein the content of the first and second substances,
the instrument conditions were: a chromatographic column: FS-SE-54-CB-0.5; column temperature: 60 ℃; carrier gas flow: 0-2min,2mL/min, 2-20min,2mL/min-100 mL/min; drift gas flow rate: 150 mL/min; carrier gas/drift gas: n is a radical of2(ii) a IMS temperature: 45 ℃; temperature of the sample injection needle: 85 ℃; sample introduction volume: 500 mu L of the solution;
2) and identifying according to the response value of the marker in the spectrogram of the to-be-detected product.
2. The method of claim 1, further comprising incubating the honey to be tested prior to feeding.
3. The method according to claim 2, wherein the incubation time is 20-30min and the incubation temperature is 55-65 ℃.
4. The method as claimed in claim 1, wherein the spectrogram to be detected obtained in step 1) is operated to obtain a representative spectrogram of a single sample, and then the representative spectrogram is subjected to maximum value normalization processing and then used as a judgment basis.
5. The method of claim 4, wherein the operations comprise background subtraction, chromatographic peak extraction and peak alignment of the data.
6. The method of claim 1, comprising the steps of:
1) weighing 2-5g of honey to be detected, placing the honey to be detected in a headspace sample injection bottle, incubating the honey to be detected, and separating the incubated honey on a gas chromatography-ion mobility spectrometer;
a chromatographic column: FS-SE-54-CB-0.5;
carrier gas flow: 0-2min,2mL/min, 2-20min,2mL/min-100 mL/min;
drift gas flow rate: 150 mL/min;
carrier gas/drift gas: n is a radical of2；
2) And identifying according to the response value of the marker in the spectrogram of the to-be-detected product.
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