CN111289644B - Method for detecting volatile components of peony living plant - Google Patents
Method for detecting volatile components of peony living plant Download PDFInfo
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Abstract
The invention relates to a method for detecting volatile components of peony living plants, which belongs to the field of plant component detection, is optimized from aspects of flower fragrance sample collection, gas chromatography-mass spectrometry conditions and the like, is suitable for qualitative and quantitative analysis of volatile components of various peony varieties under near-natural conditions, and can relatively truly reflect the volatile components and release amount of peony. The collection method is convenient to carry, simple to operate, low in cost and easy to implement, and effectively solves the three problems that the volatile components of the damaged materials are changed, samples cannot be stored for a long time and a large amount of samples cannot be simultaneously sampled in the traditional in-vitro measurement method; the self-made adsorption tube is not required to be activated by an activation instrument and the like before use, so that the time and the cost are saved; under the condition of gas chromatography-mass spectrometry, various volatile components and relative contents of peony of 'paeonia ostii' peony and other varieties can be stably and accurately detected, and the method is suitable for detecting peony flower fragrance samples collected by a dynamic headspace adsorption method.
Description
Technical Field
The invention belongs to the technical field of plant component detection, and particularly relates to a method for detecting volatile components of peony living plants.
Background
Three main ornamental features of the flower: flower type, flower color, flower fragrance. Among them, flower fragrance is known as "spiritual soul of flowers", which is one of important aesthetic indicators of ornamental plants. The fragrance released by the flowers of the plants can treat some psychological and physiological diseases, the aromatic compounds extracted from the aromatic plants have important application values in the aspects of medical treatment, health preservation, beauty treatment and the like, and the economic value of the fragrance is increasingly pursued by the public. Peony is a special aromatic plant in China as a candidate national flower, is called as the king of flowers, is reputed to be in the sea and abroad due to large, bright and fragrant flowers, and has high ornamental value.
At present, in the aspect of aromatic plants, the aroma components of plants such as China roses, narcissus, wintersweet, roses and the like are determined, but research reports on identification of volatile components of peony flowers are few, and all the research reports adopt in vitro determination methods, such as a solid phase microextraction method (SPME) and a static headspace method (SHS) and the like. The traditional in vitro measurement method can cause damage to petals and change aroma components. The dynamic headspace adsorption method is a method for sampling volatile components of living plants, and is not reported in peony fragrance component collection. Meanwhile, whether the dynamic headspace adsorption method or other detection methods are adopted, the collection of the sample is very critical. Because the peony aromatic volatile components can not be stored for a long time, the peony aromatic volatile components must be rapidly measured in a short time, otherwise, the components are lost or changed, and the accuracy of the result is influenced. And the tree peony plant type is great, and the root system is complicated, and the flowering phase is shorter, and difficult a large amount of samplings are difficult, and when the sample was gathered, because prior art's restriction, it is difficult to avoid above-mentioned problem.
The gas chromatography-mass spectrometry (GC-MS) is an effective means for analyzing and identifying volatile chemical components. In recent years, the application of GC-MS in floral research is becoming increasingly common. The volatile components of different varieties of peony are qualitatively analyzed by adopting a solid phase microextraction method (SPME) combined with a gas chromatography-mass spectrometry (GC-MS) technology, and 34 components are detected from 10 varieties of peony. Glistening et al used a Static Headspace (SHS) -gas chromatography-mass spectrometry (GC-MS) method to separate and identify 30 volatile components from 4 varieties of peony. However, different sampling methods can cause the volatile components of the flowers to have differences, and the conditions of gas chromatography-mass spectrometry are changed accordingly.
Disclosure of Invention
In order to solve the defects in the prior art, the invention aims to provide a detection method of volatile components of peony living plants, which is optimized in aspects of a flower fragrance sample collection method, gas chromatography-mass spectrometry conditions and the like, can relatively truly reflect the volatile components and relative content of peony, and is suitable for qualitative and quantitative analysis of the volatile components of various varieties of peony under near-natural conditions.
In order to achieve the purpose, the invention adopts the specific scheme that:
a method for detecting volatile components of peony living plants comprises the following steps:
step one, manufacturing an adsorption tube: taking a glass hollow tube with the outer diameter of 4-6 mm and the length of 80-100 mm, cleaning and drying; plugging the glass wool into the hollow glass tube, and filling the glass wool into the hollow glass tube to form a space of 40-60mm 3 Tenax TA ofAn adsorbent is washed by 100-200 mu L of absolute ethyl alcohol, 100-200 mu L of dichloromethane and 100-200 mu L of n-pentane in sequence to prepare an adsorption tube;
secondly, selecting peony flowers which are strong in growth, consistent in growth vigor and moderate in flower size, and respectively covering odorless and transparent sampling bags with openings at two ends; inserting an activated carbon tube at the upper end of the sampling bag, inserting an adsorption tube manufactured in the first step at the lower end of the sampling bag, and sealing the upper end and the lower end of the sampling bag by plastic clamping strips respectively;
step three, the QC-1S type atmosphere sampling instrument is erected at a proper position, the height is adjusted, a glass Y tube is connected to an air inlet, and the glass Y tube comprises a lower tube opening and two branch tube openings; the lower pipe orifice is connected with the air inlet through a tasteless transparent silicone tube; adjusting various parameters of the atmosphere sampling instrument, controlling the flow rate to be 300-600 mL/min, and controlling the collection time to be 2-4 h;
step four, respectively connecting two branch pipe orifices of the glass Y pipe with an adsorption pipe at the lower end of the peony through a tasteless transparent silicone tube, opening an atmosphere sampling instrument, and starting sampling;
step five, after sampling, taking down the adsorption tube, sealing the adsorption tube by using a preservative film, wrapping the adsorption tube by using tin foil paper, and putting the wrapped adsorption tube in an ultra-low temperature ice box to be brought back to a laboratory to finish sample collection;
sixthly, adding 500-1000 mu L of n-hexane into the adsorption tube, vertically inserting the adsorption tube into a clean brown sample injection bottle, and repeatedly pumping and beating an opening at the upper end of the adsorption tube by using an aurilave to enable the n-hexane to elute the adsorbent in the adsorption tube, thereby obtaining an eluent;
step seven, purging the eluent by nitrogen to concentrate the eluent to 200 mu L, and storing the eluent in a refrigerator at the temperature of minus 20 ℃ for later use;
step eight: and opening the gas chromatograph-mass spectrometer, setting the gas chromatography-mass spectrometry conditions, and injecting a sample for detection.
As a further optimization of the scheme, the gas chromatography-mass spectrometry conditions in the step eight are divided into gas chromatography conditions and mass spectrometry conditions;
the gas chromatography conditions were: HP-5MS elastic quartz capillary column; column flow rate: 0.8 mL/min; column temperature: the initial temperature is 70 ℃, the temperature is raised to 160 ℃ at the speed of 6 ℃/min, then the temperature is raised to 180 ℃ at the speed of 2 ℃/min, and then the temperature is raised to 250 ℃ at the speed of 5 ℃/min, and the temperature is kept for 10 min; the temperature of a sample inlet is 250 ℃; carrier gas: high-purity helium with the flow rate of 0.8 mL/min; and (3) sample introduction mode: shunting and sampling; sample introduction amount: 5 mu L of the solution;
the mass spectrum conditions are as follows: EI source: 70 eV; interface temperature: 250 ℃; the ion source temperature is 230 ℃; the temperature of the quadrupole rods is 150 ℃; EM voltage 1247V; the scan range is 29-450 amu.
Has the advantages that:
1. the dynamic headspace adsorption method selected by the invention is used as a method for collecting volatile components of living plants and is used on peony for the first time. The method can effectively solve the three defects of the traditional in vitro determination method for detecting the fragrance components of the peony flowers: firstly, after the peony petals are damaged, part of volatile components can be quickly volatilized, so that the fragrance components are changed; secondly, the collected sample must be rapidly measured in a short time and cannot be stored for a long time; thirdly, a large number of samples cannot be collected simultaneously. The method is convenient to carry, simple to operate, low in cost and easy to implement. The peony plant type is large, the root system is complex, the flowering phase is short, so that the living plant is difficult to bring back to a laboratory for sampling, the method is adopted, only the atmosphere sampling instrument, the sampling bag and various glass products are needed to be carried to a test field, the on-site sampling can be simultaneously carried out on multiple peony plants, the instrument is light, and the sampling position can be replaced at any time. The collected samples can be stored in a refrigerator at-20 deg.C for 3-6 months.
2. The peony has large flowers and moderate fragrance, and the sampling time is too long or too short, which causes the unsatisfactory effect of the sample. The method is reasonable in sampling time and suitable for collecting peony flower fragrance samples.
3. The adsorption tube used in the invention is self-made, and is not required to be activated by an activating instrument and other instruments before use, so that the time and the cost are saved, the adsorbent can be taken out and thrown away after use, and the glass tube can be reused after being cleaned, so that the method is convenient and rapid, simple to operate and easy to realize.
4. The detection technology is a gas chromatography-mass spectrometry technology, multiple volatile components in the flower fragrance samples of peony varieties such as Paeonia ostii 'peony and Paeonia suffruticosa' peony under the gas chromatography-mass spectrometry condition can be completely separated, the relative content of various components can be accurately measured, the stability is good, the accuracy is high, the detection technology is suitable for detecting the flower fragrance samples of the peony collected by a dynamic headspace adsorption method, and the detection technology can be applied to qualitative and quantitative analysis of the volatile components in the various peony varieties.
Drawings
FIG. 1 is a schematic diagram of a method for collecting volatile components of a peony living plant, namely a dynamic headspace adsorption method; the device comprises an adsorption tube, a silica gel tube, an activated carbon tube, a sampling bag, an air sampling instrument, an air inlet, an air outlet and an air flow direction, wherein A represents the activated carbon tube, B represents the sampling bag, C represents the adsorption tube, D represents the silica gel tube, E represents the glass Y tube, F represents the air sampling instrument, G represents the air inlet of the air sampling instrument, H represents the air outlet of the air sampling instrument, and I represents the air flow direction;
figure 2 is a total ion flow graph of a 'paeonia ostii' peony floral sample; wherein the abscissa is time and the ordinate is abundance;
FIG. 3 is a total ion flow graph of a 'Chunruihua House' peony floral sample; where the abscissa is time and the ordinate is abundance.
Detailed Description
A method for collecting volatile components of peony living plants comprises the following steps:
the method comprises the following steps: and (4) self-making an adsorption tube. Taking a glass adsorption hollow tube with an outer diameter of 4-6 mm and a length of 80-100 mm, cleaning, drying, plugging the glass wool removed with a special tool into the glass hollow tube, and filling into the glass hollow tube with a size of 40-60mm 3 The Tenax TA adsorbent is followed by washing the adsorption tube with 100-200. mu.L of anhydrous ethanol, 100-200. mu.L of dichloromethane and 100-200. mu.L of n-pentane. Making enough adsorption tubes by the same method, and placing in a cool and dry place for later use.
Step two: selecting strong and consistent peony flowers with moderate flower sizes, covering the selected live peony flowers with tasteless transparent sampling bags with openings at two ends respectively as shown in figure 1, inserting an active carbon tube into the upper end of each sampling bag, inserting an adsorption tube into the lower end of each sampling bag, and sealing with plastic clamping strips respectively.
Step three: and (3) placing the QC-1S type atmosphere sampling instrument frame at a proper position, adjusting the height, and connecting one end of an air inlet with a customized glass Y-shaped tube by using a tasteless transparent silicone tube. Adjusting various parameters of the atmosphere sampling instrument, controlling the flow rate to be 300-600 mL/min, and the collection time to be 2-4 h.
Step four: two branches of the glass Y tube are connected with an adsorption tube at the lower end of the peony by an odorless transparent silicone tube. And opening the atmosphere sampling instrument and starting sampling. In the sampling, the atmosphere sampling appearance begins work, the air current is by sampling bag flow direction air inlet, the air in the sampling bag lasts the output and flows through the adsorption tube, the volatile substance that the live body peony gived off is adsorbed by the adsorbent in the adsorption tube, when the air in the sampling bag lasts the outflow, the orificial air of active carbon through sampling bag upper end lasts the replenishment again, moisture and dust in the air can be disposed of to the active carbon in the active carbon pipe, in order to avoid influencing the adsorption effect of follow-up adsorbent to peony volatile smell material.
Step five: after sampling, the adsorption tube is sealed by a preservative film, then wrapped by tinfoil paper, and placed in an ultra-low temperature ice box to be brought back to a laboratory.
Step six: after the collection is finished, 500-1000 mu L of n-hexane is added into the adsorption tube, the adsorption tube is vertically inserted into a clean brown sample injection bottle, and an ear washing ball is used for repeatedly pumping and beating an opening at the upper end of the adsorption tube so that the n-hexane elutes the adsorbent in the adsorption tube to obtain an eluent.
Step seven: the eluate was purged with nitrogen and concentrated to 100-200. mu.L. The samples were stored in a freezer at-20 ℃ until they were taken out for instrumental analysis.
Step eight: the GC-MS (Agilent 6890/5973N) was turned on and the GC-MS conditions were set. And (5) manually injecting a sample for detection. (1) Gas chromatography conditions: HP-5MS (0.25 mm. times.30 m, 0.25 μm) elastic quartz capillary column; column flow rate: 0.8 mL/min; column temperature: the initial temperature is 70 ℃, the temperature is increased to 160 ℃ at the speed of 6 ℃/min, then the temperature is increased to 180 ℃ at the speed of 2 ℃/min, and then the temperature is increased to 250 ℃ at the speed of 5 ℃/min, and the temperature is kept for 10 min; the injection port temperature is 250 ℃; carrier gas: high-purity helium with the flow rate of 0.8 mL/min; and (3) sample introduction mode: shunting and sampling; sample introduction amount: 5 μ L. (2) Mass spectrum conditions: EI source: 70 eV; interface temperature: 250 ℃; the ion source temperature is 230 ℃; the temperature of the quadrupole rods is 150 ℃; EM voltage 1247V; the scan range is 29-450 amu.
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the embodiments of the present invention.
Example 1
The method comprises the following steps: and (4) self-making an adsorption tube. Taking a glass adsorption hollow tube with an outer diameter of 4-6 mm and a length of 80-100 mm, cleaning, drying, plugging the glass wool removed with a special tool into the glass hollow tube, and filling into the glass hollow tube with a size of 40-60mm 3 The Tenax TA adsorbent was followed by washing the adsorption tube with 100-. Making enough adsorption tubes by the same method, and placing in a cool and dry place for later use.
Step two: two ten-year-old Paeonia ostii' peony flowers which are robust in growth, consistent in growth vigor and moderate in flower size are selected, and are respectively covered with a sampling bag which is tasteless and transparent and is provided with openings at two ends. The upper end of the sampling bag is inserted into an activated carbon tube, and the lower end of the sampling bag is inserted into a self-made adsorption tube, which is respectively sealed by plastic clamping strips.
Step three: and (3) erecting a QC-1S type atmosphere sampling instrument at a proper position, adjusting the height, and connecting one end of an air inlet with a customized glass Y-shaped tube by using a tasteless transparent silicone tube. Adjusting various parameters of the atmosphere sampling instrument, controlling the flow rate to be 300-600 mL/min, and the collection time to be 2-4 h.
Step four: two branches of the glass Y tube are connected with the adsorption tubes at the lower ends of the two peony flowers by an odorless transparent silicone tube. And opening the atmosphere sampling instrument and starting sampling.
Step five: after sampling, the adsorption tube is sealed by a preservative film, then wrapped by tinfoil paper, and placed in an ultra-low temperature ice box to be brought back to a laboratory.
Step six: after the collection is finished, 500-1000 mu L of n-hexane is added into the adsorption tube, the adsorption tube is vertically inserted into a clean brown sample injection bottle, and an ear washing ball is used for repeatedly pumping and beating an opening at the upper end of the adsorption tube so that the n-hexane elutes the adsorbent in the adsorption tube to obtain an eluent.
Step seven: the eluate was purged with nitrogen and concentrated to 100-200. mu.L. The samples were stored in a freezer at-20 ℃ until they were taken out for instrumental analysis.
Step eight: the GC-MS (Agilent 6890/5973N) was turned on and the GC-MS conditions were set. And (5) manually injecting a sample for detection. (1) Gas chromatography conditions: HP-5MS (0.25 mm. times.30 m, 0.25 μm) elastic quartz capillary column; column flow rate: 0.8 mL/min; column temperature: the initial temperature is 70 ℃, the temperature is increased to 160 ℃ at the speed of 6 ℃/min, then the temperature is increased to 180 ℃ at the speed of 2 ℃/min, and then the temperature is increased to 250 ℃ at the speed of 5 ℃/min, and the temperature is kept for 10 min; the temperature of a sample inlet is 250 ℃; carrier gas: high-purity helium gas with the flow rate of 0.8 mL/min; and (3) sample introduction mode: shunting and sampling; sample injection amount: 5 μ L. (2) Mass spectrum conditions: EI source: 70 eV; interface temperature: 250 ℃; the ion source temperature is 230 ℃; the temperature of the quadrupole rods is 150 ℃; EM voltage 1247V; the scan range is 29-450 amu.
And (3) detection results: through mass spectrum library retrieval and manual map analysis, 23 main compounds are identified in the Paeonia ostii Paeonia suffruticosa in the initial stage, namely ocimene, undecane, dodecane, tridecane, tetradecane, 1, 3, 5-trimethoxybenzene, pentadecane, 1-hexadecene, hexadecane, cis-7-dodecen-1-ol acetate, 8-heptadecene, heptadecane, 1-octadecene, octadecane, nonadecane, dibutyl phthalate, trans-5-eicosene, isopropyl palmitate, docosane, tricosane, tetracosane, pentacosane and hexacosane, wherein the number of alkanes is 14, the number of alkenes is 5, the number of esters is 3, and the number of other compounds is 1. Undecane, dodecane, cis-7-dodecen-1-ol acetate, dibutyl phthalate, trans-5-eicosene, isopropyl palmitate, hexacosane were first determined in 'Paeonia ostii'. The relative contents are as follows: alkane compounds, ester compounds, olefin compounds and other compounds. The relative content of pentadecane in the alkane compounds is 5.245%; the ester compound has the highest relative content of the cis-7-dodecene-1-alcohol acetate, which is 1.989 percent; the relative content of 8-heptadecene in the olefin compound is the highest and is 1.454 percent.
Example 2
The method comprises the following steps: and (4) self-making an adsorption tube. Taking an outer diameterAdsorbing hollow glass tube with length of 80-100 mm and length of 4-6 mm, cleaning, oven drying, inserting the glass wool into the hollow glass tube with special tool, and filling into the hollow glass tube with length of 40-60mm 3 The Tenax TA adsorbent is followed by washing the adsorption tube with 100-200. mu.L of anhydrous ethanol, 100-200. mu.L of dichloromethane and 100-200. mu.L of n-pentane. Making enough adsorption tubes by the same method, and placing in a cool and dry place for later use.
Step two: two ten-year-old 'spring Guihua' peony plants which are robust in growth, consistent in growth vigor and moderate in flower size are selected and respectively covered with a tasteless transparent sampling bag with openings at two ends. The upper end of the sampling bag is inserted into an activated carbon tube, and the lower end of the sampling bag is inserted into a self-made adsorption tube, which is respectively sealed by plastic clamping strips.
Step three: and (3) erecting a QC-1S type atmosphere sampling instrument at a proper position, adjusting the height, and connecting one end of an air inlet with a customized glass Y-shaped tube by using a tasteless transparent silicone tube. Adjusting various parameters of the atmosphere sampling instrument, controlling the flow rate to be 300-600 mL/min, and the collection time to be 2-4 h.
Step four: two branches of the glass Y tube are connected with the adsorption tubes at the lower ends of the two peony flowers by a tasteless transparent silicone tube. And opening the atmosphere sampler and starting sampling.
Step five: after sampling, the adsorption tube is sealed by a preservative film, then wrapped by tinfoil paper, and placed in an ultra-low temperature ice box to be brought back to a laboratory.
Step six: after the collection is finished, 500-1000 mu L of n-hexane is added into the adsorption tube, the adsorption tube is vertically inserted into a clean brown sample injection bottle, and an ear washing ball is used for repeatedly pumping and beating an opening at the upper end of the adsorption tube so that the n-hexane elutes the adsorbent in the adsorption tube to obtain an eluent.
Step seven: the eluate was purged with nitrogen and concentrated to 100-200. mu.L. The samples were stored in a-20 ℃ freezer until removed for instrumental analysis.
Step eight: the GC-MS (Agilent 6890/5973N) was turned on and the GC-MS conditions were set. And (5) manually injecting a sample for detection. (1) Gas chromatography conditions: HP-5MS (0.25 mm. times.30 m, 0.25 μm) elastic quartz capillary column; column flow rate: 0.8 mL/min; column temperature: the initial temperature is 70 ℃, the temperature is increased to 160 ℃ at the speed of 6 ℃/min, then the temperature is increased to 180 ℃ at the speed of 2 ℃/min, and then the temperature is increased to 250 ℃ at the speed of 5 ℃/min, and the temperature is kept for 10 min; the injection port temperature is 250 ℃; carrier gas: high-purity helium with the flow rate of 0.8 mL/min; and (3) sample introduction mode: shunting and sampling; sample introduction amount: 5 μ L. (2) Mass spectrum conditions: EI source: 70 eV; interface temperature: 250 ℃; the ion source temperature is 230 ℃; the temperature of the quadrupole rods is 150 ℃; EM voltage 1247V; the scan range is 29-450 amu.
And (3) detection results: through mass spectrum library retrieval and manual spectrogram analysis, 22 main compounds are identified in 'Chunguhua' peony in the initial stage, namely p-dimethoxybenzene, dodecane, trans-2-tetradecene, tetradecane, pentadecane, phenol 2, 4-bis (1, 1-dimethyl), cis-7-hexadecene, hexadecane, cis-7-dodecen-1-ol acetate, 8-heptadecene, heptadecane, trans-3-octadecene, octadecane, nonadecane, dibutyl phthalate, trans-5-eicosene, eicosane, 1-docosadiene, docosane, tetracosane, pentacosane and diisooctyl phthalate, wherein 11 alkanes, 6 alkenes, 3 esters and 2 other compounds are respectively identified. The relative contents are as follows: alkane compounds, olefin compounds, ester compounds and other compounds. The relative content of hexadecane in the alkane compound is 6.355%; the relative content of trans-3-octadecene in the olefin compounds is 6.297 percent; the highest cis-7-dodecene-1-ol acetate content in the ester compound is 6.547%.
It should be noted that the above-mentioned embodiments illustrate rather than limit the scope of the invention, which is defined by the appended claims. It will be apparent to those skilled in the art that certain insubstantial modifications and adaptations of the present invention can be made without departing from the spirit and scope of the invention.
Claims (1)
1. A detection method of volatile components of peony living plants is characterized by comprising the following steps: the method comprises the following steps:
step one, manufacturing an adsorption tube: taking a branch with an outer diameter of 4-6 mmCleaning and drying the glass hollow tube with the length of 80-100 mm; plugging the glass wool into the hollow glass tube, and filling the glass wool into the hollow glass tube to form a space with a diameter of 40-60mm 3 Then sequentially washing with 100-200 mu L absolute ethyl alcohol, 100-200 mu L dichloromethane and 100-200 mu L n-pentane to prepare an adsorption tube;
secondly, selecting peony flowers which are strong in growth, consistent in growth vigor and moderate in flower size, and respectively covering odorless and transparent sampling bags with openings at two ends; inserting an active carbon tube at the upper end of the sampling bag, inserting an adsorption tube manufactured in the first step at the lower end of the sampling bag, and sealing the upper end and the lower end of the sampling bag by plastic clamping strips respectively;
step three, the QC-1S type atmosphere sampling instrument is erected at a proper position, the height is adjusted, a glass Y tube is connected to an air inlet, and the glass Y tube comprises a lower tube opening and two branch tube openings; the lower pipe orifice is connected with the air inlet through a tasteless transparent silicone tube; adjusting various parameters of the atmosphere sampling instrument, controlling the flow rate to be 300-600 mL/min, and controlling the collection time to be 2-4 h;
step four, respectively connecting two branch pipe orifices of the glass Y pipe with an adsorption pipe at the lower end of the peony through a tasteless transparent silicone tube, opening an atmosphere sampling instrument, and starting sampling;
step five, after sampling, taking down the adsorption tube, sealing the adsorption tube by using a preservative film, wrapping the adsorption tube by using tin foil paper, and putting the wrapped adsorption tube in an ultra-low temperature ice box to be brought back to a laboratory to finish sample collection;
step six, adding 500-1000 mu L of normal hexane into the adsorption tube, vertically inserting the adsorption tube into a clean brown sample injection bottle, and repeatedly pumping an opening at the upper end of the adsorption tube by using an aurilave so that the normal hexane elutes the adsorbent in the adsorption tube to obtain an eluent;
step seven, purging the eluent by nitrogen to concentrate the eluent to 200 mu L, and storing the eluent in a refrigerator at the temperature of minus 20 ℃ for later use;
step eight: opening a gas chromatograph-mass spectrometer, setting gas chromatography-mass spectrometry conditions, and carrying out sample injection for detection;
step eight, dividing the gas chromatography-mass spectrometry conditions into gas chromatography conditions and mass spectrometry conditions;
the gas chromatography conditions were: HP-5MS elastic quartz capillary column; column flow rate: 0.8 mL/min; column temperature: the initial temperature is 70 ℃, the temperature is increased to 160 ℃ at the speed of 6 ℃/min, then the temperature is increased to 180 ℃ at the speed of 2 ℃/min, and then the temperature is increased to 250 ℃ at the speed of 5 ℃/min, and the temperature is kept for 10 min; the temperature of a sample inlet is 250 ℃; carrier gas: high-purity helium with the flow rate of 0.8 mL/min; and (3) sample introduction mode: split-flow sample injection; sample introduction amount: 5 mu L of the solution; the specification of the HP-5MS elastic quartz capillary column is 0.25 mm multiplied by 30 m and 0.25 mu m;
the mass spectrum conditions are as follows: EI source: 70 eV; interface temperature: 250 ℃; the ion source temperature is 230 ℃; the temperature of the quadrupole rods is 150 ℃; EM voltage 1247V; the scanning range is 29-450 amu;
through mass spectrum library retrieval and manual map analysis, 23 compounds are identified in the Paeonia ostii Paeonia suffruticosa in the initial stage, wherein the 23 compounds are ocimene, undecane, dodecane, tridecane, tetradecane, 1, 3, 5-trimethoxybenzene, pentadecane, 1-hexadecene, hexadecane, cis-7-dodecen-1-ol acetate, 8-heptadecene, heptadecane, 1-octadecene, octadecane, nonadecane, dibutyl phthalate, trans-5-eicosene, isopropyl palmitate, docosane, tricosane, tetracosane, pentacosane and hexacosane respectively;
through mass spectrum library retrieval and manual spectrogram analysis, 22 compounds are identified in 'Chunguhua' peony in the initial stage, namely p-dimethoxybenzene, dodecane, trans-2-tetradecene, tetradecane, pentadecane, phenol 2, 4-bis (1, 1-dimethyl), cis-7-hexadecene, hexadecane, cis-7-dodecen-1-ol acetate, 8-heptadecene, heptadecane, trans-3-octadecene, octadecane, nonadecane, dibutyl phthalate, trans-5-eicosene, eicosane, 1-docosadiene, docosane, tetracosane, pentacosane and diisooctyl phthalate.
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Application publication date: 20200616 Assignee: Sanmenxia Muxian Biotechnology Co.,Ltd. Assignor: HENAN University OF SCIENCE AND TECHNOLOGY Contract record no.: X2023980041891 Denomination of invention: A Method for Detecting Volatile Components in Living Plants of Peony Granted publication date: 20220830 License type: Common License Record date: 20230920 |