CN111398501A - Method for determining content of sex pheromone in tobacco beetle sex pheromone lure core - Google Patents

Method for determining content of sex pheromone in tobacco beetle sex pheromone lure core Download PDF

Info

Publication number
CN111398501A
CN111398501A CN202010205592.6A CN202010205592A CN111398501A CN 111398501 A CN111398501 A CN 111398501A CN 202010205592 A CN202010205592 A CN 202010205592A CN 111398501 A CN111398501 A CN 111398501A
Authority
CN
China
Prior art keywords
sex pheromone
temperature
trap
tobacco beetle
tobacco
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Granted
Application number
CN202010205592.6A
Other languages
Chinese (zh)
Other versions
CN111398501B (en
Inventor
黄惠贞
张建平
刘秀彩
谢卫
李巧灵
张鼎方
刘泽春
梁晖
林艳
黄华发
周培琛
黄朝章
许寒春
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
China Tobacco Fujian Industrial Co Ltd
Original Assignee
China Tobacco Fujian Industrial Co Ltd
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by China Tobacco Fujian Industrial Co Ltd filed Critical China Tobacco Fujian Industrial Co Ltd
Priority to CN202010205592.6A priority Critical patent/CN111398501B/en
Publication of CN111398501A publication Critical patent/CN111398501A/en
Application granted granted Critical
Publication of CN111398501B publication Critical patent/CN111398501B/en
Active legal-status Critical Current
Anticipated expiration legal-status Critical

Links

Images

Classifications

    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N30/00Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
    • G01N30/02Column chromatography
    • G01N30/88Integrated analysis systems specially adapted therefor, not covered by a single one of the groups G01N30/04 - G01N30/86
    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N30/00Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
    • G01N30/02Column chromatography
    • G01N30/88Integrated analysis systems specially adapted therefor, not covered by a single one of the groups G01N30/04 - G01N30/86
    • G01N2030/8809Integrated analysis systems specially adapted therefor, not covered by a single one of the groups G01N30/04 - G01N30/86 analysis specially adapted for the sample
    • G01N2030/8813Integrated analysis systems specially adapted therefor, not covered by a single one of the groups G01N30/04 - G01N30/86 analysis specially adapted for the sample biological materials

Landscapes

  • Physics & Mathematics (AREA)
  • Health & Medical Sciences (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Chemical & Material Sciences (AREA)
  • Analytical Chemistry (AREA)
  • Biochemistry (AREA)
  • General Health & Medical Sciences (AREA)
  • General Physics & Mathematics (AREA)
  • Immunology (AREA)
  • Pathology (AREA)
  • Other Investigation Or Analysis Of Materials By Electrical Means (AREA)

Abstract

The invention belongs to the field of detection and analysis, and particularly relates to a method for determining the content of sex pheromone in a tobacco beetle sex pheromone lure, which comprises the following steps: (1) immersing the tobacco beetle sex pheromone lure core by using a solvent to obtain a mixture; wherein the solvent is ethanol containing sodium borohydride, and the mass of the sodium borohydride accounts for 0.05-1% of the mass of the solvent; (2) introducing the mixture into a gas chromatography-triple quadrupole mass spectrometer through a headspace sampler with a trap, and then detecting to obtain a detection result; it also discloses specific operating conditions for the headspace sampler with trap. The method for determining the tobacco beetle sex pheromone content in the tobacco beetle sex pheromone lure and the tobacco beetle sex pheromone trap has the advantages of good repeatability, high sensitivity, low detection limit and high accuracy.

Description

Method for determining content of sex pheromone in tobacco beetle sex pheromone lure core
Technical Field
The invention belongs to the field of detection and analysis, and particularly relates to a method for determining the content of sex pheromone in a tobacco beetle sex pheromone lure core.
Background
The tobacco beetle belongs to the family of Coleoptera larkspuridae and is one of the main pests in tobacco storage warehouses in China. The tobacco beetles are wide in distribution, large in breeding amount and serious in harm, not only can eat tobacco leaves to form holes, so that the tobacco leaf shredding rate is influenced, but also a large amount of excrement is discharged, and insect corpses are left, so that the tobacco leaves are damaged in taste and the quality is reduced. The tobacco beetles cause serious loss in the tobacco industry, and according to rough estimation, the direct economic loss caused by the tobacco beetles in China reaches over 10 hundred million yuan each year.
At present, the tobacco beetle control mainly comprises the steps of monitoring the distribution and the density of the tobacco beetles by using a tobacco beetle sex pheromone trapper, killing the tobacco beetles or intervening and inhibiting the propagation of the tobacco beetles; the auxiliary prevention and treatment can be carried out by cooperating with phosphine fumigation and making good cleanness and sanitation at ordinary times.
The main component in the tobacco beetle sex pheromone trap is a tobacco beetle sex pheromone lure. Generally, the tobacco beetle sex pheromone lure core comprises a plurality of components such as tobacco beetle sex pheromone, a carrier, a synergist, a pesticide (an infertility agent), a synergist, a diluent, a slow release agent and the like, and some lure cores are also added with a plant-source attractant, an artificial attractant and the like. The tobacco beetle sex pheromone mainly comprises 4, 6-dimethyl-7-hydroxy-3-nonanone (6-Serricornin), wherein C7The configuration of S, namely (7S) - (mono) -4, 6-dimethyl-7-hydroxy-3-nonanone, has stronger sexual induction activity. The content and the content stability of the tobacco beetle sex pheromone in the tobacco beetle sex pheromone lure have important influence on the effectiveness of the trap, so that the content of the tobacco beetle sex pheromone in the tobacco beetle sex pheromone lure needs to be accurately known, however, the components in the tobacco beetle sex pheromone lure are complex and various, and a common detection method (such as GC-MS) cannot accurately determine the content of the tobacco beetle sex pheromone in the lure. Therefore, a method for accurately detecting the content of the sex pheromone of the tobacco beetles in the tobacco beetle sex pheromone lure is urgently needed.
Disclosure of Invention
The invention provides a method for determining the content of sex pheromone in a tobacco beetle sex pheromone lure core, which adopts a certain solvent for extraction, accurately determines the content of the sex pheromone in the lure core by a headspace sample injector with a trap and a gas chromatography-triple quadrupole mass spectrometer and by using a certain detection condition, and has the advantages of good repeatability, high sensitivity, low detection limit and high accuracy. On the basis, the invention also provides a method for determining the content of the sex pheromone in the sex pheromone trap of the tobacco beetles.
The invention relates to a method for determining the content of (tobacco beetle) sex pheromone in a tobacco beetle sex pheromone lure, which comprises the following steps:
(1) immersing the tobacco beetle sex pheromone lure core by using a solvent to obtain a mixture; wherein the solvent is ethanol containing sodium borohydride, and the mass of the sodium borohydride accounts for 0.05-1% of the mass of the solvent, such as 0.06%, 0.07%, 0.08%, 0.09%, 0.1%, 0.15%, 0.2%, 0.3%, 0.4%, 0.5%, 0.7%, 1%;
(2) introducing the mixture into a gas chromatography-triple quadrupole mass spectrometer through a headspace sampler with a trap, and then detecting to obtain a detection result;
wherein the operating conditions of the trap-equipped headspace sampler comprise:
a heating equilibrium temperature of 70 to 80 ℃ (e.g., 72 ℃, 75 ℃, 78 ℃), a heating equilibrium time of 20 to 40 minutes (e.g., 25 minutes, 30 minutes), a needle temperature of 90 to 100 ℃ (e.g., 93 ℃, 95 ℃, 98 ℃), a transfer line temperature of 105 to 125 ℃ (e.g., 110 ℃, 115 ℃, 120 ℃), a trap low temperature of-55 to-25 ℃ (e.g., -50 ℃, 45 ℃, 40 ℃, 35 ℃, 32 ℃, 30 ℃), a trap high temperature of 160 to 200 ℃ (e.g., 165 ℃, 170 ℃, 175 ℃, 180 ℃, 185 ℃, 190 ℃, 195 ℃), a desorption time of 0.1 to 2 minutes (e.g., 0.5 minute, 1 minute, 1.5 minutes), a desorption pressure of 25 to 45Psi (e.g., 30Psi, 35Psi, 40Psi), a bottle pressure of 30 to 50Psi (e.g., 35Psi, 40Psi, 45Psi), the column pressure is 20 to 50Psi (e.g., 30Psi, 35Psi, 40Psi, 45Psi), the trap hold time is 1 to 10 minutes (e.g., 2, 5, 7, 8 minutes), and the dry purge time is 0.5 to 8 minutes (e.g., 1, 2, 3, 5, 7 minutes).
In some embodiments of the first aspect of the present invention, the headspace sampler with trap does not shunt during operation.
In some embodiments of the first aspect of the present invention, the (tobacco beetle) sex pheromone is 4, 6-dimethyl-7-hydroxy-3-nonanone, preferably (7S) - (mono) -4, 6-dimethyl-7-hydroxy-3-nonanone.
In certain embodiments of the first aspect of the present invention, in step (1), the mass of sodium borohydride is 0.05% to 0.4% of the mass of solvent.
In certain embodiments of the first aspect of the present invention, in step (1), the volume of solvent is sufficient to submerge the tobacco beetle sex pheromone attractant core.
In some embodiments of the first aspect of the present invention, the solvent is anhydrous ethanol containing sodium borohydride, which is also understood to be a mixture of sodium borohydride and anhydrous ethanol.
In certain embodiments of the first aspect of the present invention, in step (2), the operating conditions of the gas chromatograph comprise one or more of the following a to G:
A. the chromatographic column is HP-5MS (UI) column;
preferably, the HP-5MS (UI) column is a capillary column;
B. the specification of the chromatographic column is 60m × 0.25mm,0.25 μm;
C. the carrier gas is helium;
D. the injection port temperature is 80-120 deg.C, such as 85 deg.C, 90 deg.C, 95 deg.C, 100 deg.C, 105 deg.C, 110 deg.C, 115 deg.C;
E. a constant pressure mode is adopted;
F. the temperature rising program of the chromatographic column is as follows: 30 to 50 ℃ (e.g., 35 ℃, 40 ℃, 45 ℃) for 1 to 5 minutes (e.g., 2, 3, 4 minutes), 5 to 12 ℃/min (e.g., 6 ℃/min, 8 ℃/min, 10 ℃/min) up to 110 to 130 ℃ (e.g., 115 ℃, 120 ℃, 125 ℃), 110 to 130 ℃ (e.g., 115 ℃, 120 ℃, 125 ℃) up to 150 to 175 ℃ (e.g., 155 ℃, 160 ℃, 170 ℃) and 1 to 6 ℃/min (e.g., 2 ℃/min, 4 ℃/min, 5 ℃/min), then 40 to 60 ℃/min (e.g., 45 ℃/min, 50 ℃/min, 55 ℃/min) up to 250 ℃ to 270 ℃ (e.g., 255 ℃, 260 ℃, 265 ℃), 250 to 270 ℃ (e.g., 255 ℃, 260 ℃, °, Keeping the temperature at 265 ℃ for 1-10 minutes (for example, 2, 3, 4,6 and 8 minutes) and then finishing;
G. the temperature of the auxiliary heater is 250 ℃ to 290 ℃, for example 260 ℃, 270 ℃, 280 ℃.
In certain embodiments of the first aspect of the present invention, in step (2), the operating conditions of the triple quadrupole mass spectrometry comprise one or more of the following a to d:
a. the ion source temperature is 240 ℃ to 260 ℃, such as 245 ℃, 250 ℃, 255 ℃;
b. the quadrupole rods are at a temperature of 140 ℃ to 160 ℃, e.g., 145 ℃, 150 ℃, 155 ℃;
c. the ionization energy is 60-80 eV, such as 65eV, 70eV, 75 eV;
d. the scanning range is 29-350 amu.
In some embodiments of the first aspect of the present invention, the qualitative ion of (7S) - (mono) -4, 6-dimethyl-7-hydroxy-3-nonanone is 55.
In some embodiments of the first aspect of the present invention, the counterion of (7S) - (mono) -4, 6-dimethyl-7-hydroxy-3-nonanone is 86.
In some embodiments of the first aspect of the present invention, in step (2), the detection result is obtained by external standard quantitative analysis.
In a second aspect the present invention relates to a method of determining the content of (tobacco beetle) sex pheromone in a tobacco beetle sex pheromone trap, comprising the steps of:
measuring the (tobacco beetle) sex pheromone content in the tobacco beetle sex pheromone lure according to the method of the first aspect of the invention;
and calculating the content of the sex pheromone in the tobacco beetle sex pheromone trapper according to the content of the (tobacco beetle) sex pheromone in the tobacco beetle sex pheromone trapper and the quantity of the trappers in the tobacco beetle sex pheromone trapper.
In some embodiments of the second aspect of the present invention, the (tobacco beetle) sex pheromone is 4, 6-dimethyl-7-hydroxy-3-nonanone, preferably (7S) - (mono) -4, 6-dimethyl-7-hydroxy-3-nonanone.
In the invention, the tobacco beetle sex pheromone lure or the tobacco beetle sex pheromone trap are conventional commodities in the field and can be obtained commercially.
The invention has the following beneficial effects:
the method for determining the content of the sex pheromone (such as (7S) - (one) -4, 6-dimethyl-7-hydroxy-3-nonanone) of the tobacco beetles in the tobacco beetle sex pheromone lure core and the tobacco beetle sex pheromone trap has the advantages of good repeatability, high sensitivity, low detection limit and high accuracy.
Drawings
In order that the present disclosure may be more readily and clearly understood, reference is now made to the following detailed description of the embodiments of the present disclosure taken in conjunction with the accompanying drawings, in which
FIG. 1 is a chromatogram of a sample obtained in step (2) of example 1.
Detailed Description
Embodiments of the present invention will now be described more fully hereinafter with reference to the accompanying examples, in which some, but not all embodiments of the invention are shown. The following description of at least one exemplary embodiment is merely illustrative in nature and is in no way intended to limit the invention, its application, or uses. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Example 1
(1) Preparing a series of standard solutions:
adding 25mg (accurate to 0.1mg) of (7S) - (one) -4, 6-dimethyl-7-hydroxy-3-nonanone standard substance accurately weighed into a 10m L volumetric flask, adding ethanol containing 0.1% (mass concentration) of sodium borohydride for constant volume to obtain a 1-grade standard solution with the concentration of (7S) - (one) -4, 6-dimethyl-7-hydroxy-3-nonanone being 2500 mu g/m L, respectively transferring 1-grade standard solutions of 5m L, 2m L, 1m L and 0.2m L into a 10m L volumetric flask, and using ethanol containing 0.1% (mass concentration) of sodium borohydride for constant volume to prepare a 2-5-grade standard solution.
(2) Pretreatment:
putting the newly opened tobacco beetle sex pheromone lure 1 into a 20m L headspace bottle, adding 1ml of ethanol containing 0.1% (mass concentration) of sodium borohydride to immerse the lure, obtaining a sample, and sealing for later use.
(3) And (3) detection:
introducing the series of standard solutions and the sample obtained in the step (2) into a gas chromatograph-triple quadrupole mass spectrometer (Agilent 7890B gas chromatograph and Agilent 5977A MS) through a headspace sampler (Perkin Elmer Turbomatrix HST-40 headspace sampler) with a trap for detection; wherein the content of the first and second substances,
the operating conditions of the trap-equipped headspace sampler include:
the heating equilibrium temperature is 75 ℃; the heating balance time is 30 min; the temperature of the sample injection needle is 95 ℃; the temperature of the transmission line is 115 ℃; the low temperature of the trap is-40 ℃; the high temperature (desorption temperature) of the trap is 180 ℃; the desorption time is 0.5 min; the desorption pressure was 35 Psi; the bottle pressure was 40 Psi; the column pressure was 35 Psi; the retention time of the trap is 5.0 min; the dry purging time is 3.0 min; no flow split.
The operating conditions of the gas chromatograph include:
the chromatographic column is a capillary column HP-5MS (UI) column (60m × 0.25.25 mm,0.25 μm), the carrier gas is helium, the injection port temperature is 100 ℃, the constant pressure mode is adopted, the temperature of the chromatographic column is increased by maintaining for 2min at 40 ℃, increasing the temperature to 120 ℃ at the speed of 8 ℃/min, maintaining for 2min at 120 ℃, increasing the temperature to 160 ℃ at the speed of 2 ℃/min, increasing the temperature to 260 ℃ at the speed of 50 ℃/min, maintaining for 4min at 260 ℃, and the temperature of the auxiliary heater is 270 ℃;
the operating conditions of the mass spectrometer include:
the ion source temperature is 250 ℃; the temperature of the quadrupole rods is 150 ℃; ionization energy is 70 eV; the scanning range is 29-350 amu; the qualitative ion of (7S) - (one) -4, 6-dimethyl-7-hydroxy-3-nonanone was 55, and the quantitative ion was 86.
The chromatogram of the sample in step (2) is shown in FIG. 1 (1 represents the peak of the compound of (7S) - (mono) -4, 6-dimethyl-7-hydroxy-3-nonanone).
(4) Data processing:
drawing a concentration-quantitative ion peak area standard working curve Y which is 0.6237x +0.0021 (R) according to the concentration of the series of standard solutions and the measured quantitative ion peak area2=0.997). And calculating by combining the quantitative ion peak area of the sample to obtain the content of the effective component (7S) - (one) -4, 6-dimethyl-7-hydroxy-3-nonanone in the tobacco beetle sex pheromone lure 1 of 595.11 mu g/piece.
Example 2
The content of (7S) - (mono) -4, 6-dimethyl-7-hydroxy-3-nonanone in tobacco beetle sex pheromone wicks 2-13 was measured according to the method of example 1, wherein wicks 2-6 were freshly opened and the remainder were wicks left for a certain period of time after opening, and the results are shown in Table 1.
TABLE 1 measurement results
Content of (7S) - (one) -4, 6-dimethyl-7-hydroxy-3-nonanone (. mu.g/one)
Lure core 2 550.50
Lure core 3 554.64
Lure 4 515.39
Lure 5 635.96
Lure core 6 302.46
Lure core 7 54.48
Lure 8 39.43
Lure 9 36.62
Lure 10 36.29
Lure 11 36.19
Lure 12 36.08
Lure 13 36.45
As can be seen from Table 1, the sex pheromone content of the lure which was just unsealed was high; after the lure is unsealed for a period of time, the content of the sex pheromone in the lure is obviously reduced, which seriously influences the effectiveness of the lure. Therefore, it is necessary to determine and monitor the sex pheromone content of the lure.
Example 3 reproducibility, recovery, detection limit and quantitation limit of the method
The sample injection detection was repeated ten times according to the method in example 1 for the 5 th standard solution in example 1, and three times and ten times of the deviation were taken as the detection limit and the quantification limit, respectively, as shown in table 2.
On the basis of the lure 1 in example 1, 500 μ g of (7S) - (one) -4, 6-dimethyl-7-hydroxy-3-nonanone standard substance is added to obtain a standard sample, then the standard sample is subjected to pretreatment, detection and data processing according to the steps (2) - (4) in example 1, the recovery rate is calculated, and the experiment is repeated in parallel for six times, and the result is shown in table 2.
TABLE 2 repeatability, recovery, detection limit and quantitation limit results for the methods of the invention
Figure BDA0002420941730000081
As can be seen from Table 2, the relative standard deviation of the detection result of the method of the invention is less than 5%, both the detection limit and the quantification limit are low, and the recovery rate is within the normal acceptable range of 80-120%, which shows that the method of the invention has good repeatability, high sensitivity and high accuracy.
Comparative example 1
The detection method comprises the following steps: directly feeding sample into a gas chromatography-triple quadrupole mass spectrometer (Agilent 7890B gas chromatograph and Agilent 5977A MS) for detection (without feeding sample through a headspace sampler with a trap); the operating conditions and other operations of the gas chromatography and the triple quadrupole mass spectrometry were the same as those of example 1.
And (3) detecting the 1 st to 5 th-level standard solutions in the example 1 according to the detection method, and drawing a standard working curve according to the concentrations of the series of standard solutions and the measured quantitative ion peak areas. The test was repeated ten times for the grade 5 standard solution, and three times and ten times the deviation were taken as the detection limit and the quantification limit, respectively, as shown in table 3.
To the spiked sample of example 3, 1m L of 0.1% (by mass) ethanol containing sodium borohydride was added to immerse the sample, followed by testing according to the "test method" described above, data processing was performed in conjunction with the standard working curve described above, and the recovery was calculated and repeated in parallel six times, with the results shown in Table 3.
TABLE 3 results of repeatability, recovery, detection limit and quantitation limit for the method of comparative example 1
Figure BDA0002420941730000091
As can be seen from tables 2 to 3, the detection limit and the quantification limit of the method of comparative example 1 are respectively more than three times that of the method of the present invention, the relative standard deviation of the method of comparative example 1 is larger than that of the method of the present invention, and the recovery rate of the method of comparative example 1 exceeds the generally acceptable range of 80% to 120%, which indicates that the method of the present invention has better reproducibility, lower detection limit, higher sensitivity and higher accuracy compared with the method of comparative example 1.
Comparative example 2
(1) Preparing a series of standard solutions:
adding 25mg (accurate to 0.1mg) of (7S) - (one) -4, 6-dimethyl-7-hydroxy-3-nonanone standard substance accurately weighed into a 10m L volumetric flask, adding absolute ethyl alcohol for constant volume to obtain a 1-grade standard solution with the concentration of (7S) - (one) -4, 6-dimethyl-7-hydroxy-3-nonanone being 2500 mu g/m L, respectively transferring 1-grade standard solutions of 5m L, 2m L, 1m L and 0.2m L into a 10m L volumetric flask, and using absolute ethyl alcohol for constant volume to prepare a 2-5-grade standard solution.
(2) Pretreatment:
putting the newly opened tobacco beetle sex pheromone lure core 1 into a 20m L headspace bottle, adding 1ml of absolute ethyl alcohol to immerse the lure core to obtain a sample to be detected, and sealing for later use.
Putting a newly opened tobacco beetle sex pheromone lure 1 into a 20m L headspace bottle, adding 500 μ g of (7S) - (mono) -4, 6-dimethyl-7-hydroxy-3-nonanone standard substance, adding 1m L absolute ethyl alcohol to immerse all substances to obtain a standard sample, and sealing for later use.
(3) And (3) detection: and (3) taking the 1 st-5 th-level standard solution, the sample to be detected and the standard sample to be detected to perform detection according to the step (3) in the embodiment 1.
And drawing a standard working curve according to the concentration of the series of standard solutions and the measured peak area of the quantitative ion. The test was repeated ten times for the grade 5 standard solution, and three times and ten times the deviation were taken as the detection limit and the quantification limit, respectively, as shown in table 4. And (3) carrying out data processing according to the peak areas of the quantitative ions measured by the sample to be measured and the standard sample and the standard working curve, calculating the recovery rate, and repeating the experiment for six times in parallel, wherein the results are shown in Table 4.
TABLE 4 results of repeatability, recovery, detection limit and quantitation limit for the method of comparative example 2
Figure BDA0002420941730000101
As can be seen from tables 2 and 4, the relative standard deviation of the method of comparative example 2 is more than three times that of the method of the present invention, the detection limit and the quantitative limit of the method of comparative example 2 are both significantly higher than those of the method of the present invention, and the recovery rate of the method of comparative example 2 exceeds the generally acceptable range of 80% to 120%, which indicates that the method of the present invention has better repeatability, lower detection limit, higher sensitivity and higher accuracy compared with the method of comparative example 2.
It should be understood that the above examples are only for clarity of illustration and are not intended to limit the embodiments. Other variations and modifications will be apparent to persons skilled in the art in light of the above description. And are neither required nor exhaustive of all embodiments. And obvious variations or modifications therefrom are within the scope of the invention.

Claims (10)

1. A method for determining the content of sex pheromone in a sex pheromone lure of tobacco beetles comprises the following steps:
(1) immersing the tobacco beetle sex pheromone lure core by using a solvent to obtain a mixture; wherein the solvent is ethanol containing sodium borohydride, and the mass of the sodium borohydride accounts for 0.05-1% of the mass of the solvent;
(2) introducing the mixture into a gas chromatography-triple quadrupole mass spectrometer through a headspace sampler with a trap, and then detecting to obtain a detection result;
wherein the operating conditions of the trap-equipped headspace sampler comprise:
the heating balance temperature is 70-80 ℃, the heating balance time is 20-40 minutes, the temperature of a sample injection needle is 90-100 ℃, the temperature of a transmission line is 105-125 ℃, the low temperature of a trap is-55-25 ℃, the high temperature of the trap is 160-200 ℃, the desorption time is 0.1-2 minutes, the desorption pressure is 25-45 Psi, the bottle pressure is 30-50 Psi, the pressure of a chromatographic column is 20-50 Psi, the holding time of the trap is 1-10 minutes, and the dry purging time is 0.5-8 minutes.
2. The method of claim 1, wherein the sex pheromone is 4, 6-dimethyl-7-hydroxy-3-nonanone.
3. The method of claim 1, wherein the sex pheromone is (7S) - (mono) -4, 6-dimethyl-7-hydroxy-3-nonanone.
4. The method according to claim 1, wherein in the step (1), the mass of the sodium borohydride accounts for 0.05-0.4% of the mass of the solvent.
5. The method of claim 1, wherein in step (2), the trapped-band headspace sampler is not shunted during operation.
6. The method of claim 1, wherein in step (2), the operating conditions of the gas chromatograph comprise one or more of the following A to G:
A. the chromatographic column is HP-5MS (UI) column;
B. the specification of the chromatographic column is 60m × 0.25mm,0.25 μm;
C. the carrier gas is helium;
D. the temperature of a sample inlet is 80-120 ℃;
E. a constant pressure mode is adopted;
F. the temperature rising program of the chromatographic column is as follows: keeping the temperature at 30-50 ℃ for 1-5 minutes, raising the temperature to 110-130 ℃ at the speed of 5-12 ℃/min, keeping the temperature at 110-130 ℃ for 1-5 minutes, raising the temperature to 150-175 ℃ at the speed of 1-6 ℃/min, raising the temperature to 250-270 ℃ at the speed of 40-60 ℃/min, keeping the temperature at 250-270 ℃ for 1-10 minutes, and finishing;
G. the temperature of the auxiliary heater is 250-290 ℃.
7. The method of any one of claims 1 to 6, wherein in step (2), the operating conditions of triple quadrupole mass spectrometry comprise one or more of the following a to d:
a. the temperature of the ion source is 240-260 ℃;
b. the temperature of the quadrupole rods is 140-160 ℃;
c. the ionization energy is 60-80 eV;
d. the scanning range is 29-350 amu.
8. The method of claim 1, wherein in step (1), the volume of solvent is just sufficient to submerge the tobacco beetle sex pheromone attractant core.
9. The method according to claim 1, wherein in the step (2), the detection result is obtained by an external standard quantitative analysis method.
10. A method of determining the sex pheromone content in a tobacco beetle sex pheromone trap comprising the steps of:
measuring the sex pheromone content in the sex pheromone attractant core of the tobacco beetles according to the method of any one of claims 1 to 9;
and calculating the content of the sex pheromone in the tobacco beetle sex pheromone trap according to the content of the sex pheromone in the tobacco beetle sex pheromone trap and the number of the trap cores in the tobacco beetle sex pheromone trap.
CN202010205592.6A 2020-03-23 2020-03-23 Method for determining content of sex pheromone in tobacco beetle sex pheromone lure core Active CN111398501B (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CN202010205592.6A CN111398501B (en) 2020-03-23 2020-03-23 Method for determining content of sex pheromone in tobacco beetle sex pheromone lure core

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CN202010205592.6A CN111398501B (en) 2020-03-23 2020-03-23 Method for determining content of sex pheromone in tobacco beetle sex pheromone lure core

Publications (2)

Publication Number Publication Date
CN111398501A true CN111398501A (en) 2020-07-10
CN111398501B CN111398501B (en) 2022-08-30

Family

ID=71436464

Family Applications (1)

Application Number Title Priority Date Filing Date
CN202010205592.6A Active CN111398501B (en) 2020-03-23 2020-03-23 Method for determining content of sex pheromone in tobacco beetle sex pheromone lure core

Country Status (1)

Country Link
CN (1) CN111398501B (en)

Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN114062538A (en) * 2021-11-03 2022-02-18 莆田海关综合技术服务中心 Agilawood GC-MS fingerprint spectrum construction method
CN114814021A (en) * 2022-04-21 2022-07-29 浙江省化工产品质量检验站有限公司 Detection method and application of sex pheromone pesticide of ostrinia furnacalis
CN114062538B (en) * 2021-11-03 2024-05-10 莆田海关综合技术服务中心 Construction method of agilawood GC-MS fingerprint

Citations (9)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US4034080A (en) * 1976-01-14 1977-07-05 The United States Of America As Represented By The Secretary Of Agriculture Chemical attractant for smaller European bark beetle
US4317836A (en) * 1979-03-28 1982-03-02 The Japan Tobacco & Salt Public Corporation 4-6-Dimethyl-7-keto-nonan-3-ol and sex attractant comprising the same
EP0053756A1 (en) * 1980-12-05 1982-06-16 B.A.T. Cigarettenfabriken GmbH 2,6-Diethyl-3,5-dimethyl-2,3-dihydro-4H-pyran, process for its preparation and its use in the early identification and location of and in combating Lasioderma serricorne F
EP0367598A2 (en) * 1988-11-02 1990-05-09 Philip Morris Products Inc. Novel process for the production of 4,6-dimethyl-7-hydroxynonan-3-one
CN102258000A (en) * 2011-04-11 2011-11-30 李翊玮 Safe and environmentally-friendly method for preventing and controlling cigarette beetle in cigarette factory
CN104430330A (en) * 2013-09-15 2015-03-25 苏州研迪智能科技有限公司 Lure core for prevention and control of cigarette beetles
CN104914184A (en) * 2015-06-05 2015-09-16 广西中烟工业有限责任公司 Cold trap capturing-gas chromatography/mass spectrum combined detection method for furan in cigarette mainstream smoke
CN105981722A (en) * 2015-03-04 2016-10-05 温州医科大学 Lasioderma serricorne (fabricius) sex pheromone and lure thereof
CN108353901A (en) * 2018-02-02 2018-08-03 武汉东昌仓贮技术有限公司 A kind of attractant and lure for luring control cigarette beetle

Patent Citations (9)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US4034080A (en) * 1976-01-14 1977-07-05 The United States Of America As Represented By The Secretary Of Agriculture Chemical attractant for smaller European bark beetle
US4317836A (en) * 1979-03-28 1982-03-02 The Japan Tobacco & Salt Public Corporation 4-6-Dimethyl-7-keto-nonan-3-ol and sex attractant comprising the same
EP0053756A1 (en) * 1980-12-05 1982-06-16 B.A.T. Cigarettenfabriken GmbH 2,6-Diethyl-3,5-dimethyl-2,3-dihydro-4H-pyran, process for its preparation and its use in the early identification and location of and in combating Lasioderma serricorne F
EP0367598A2 (en) * 1988-11-02 1990-05-09 Philip Morris Products Inc. Novel process for the production of 4,6-dimethyl-7-hydroxynonan-3-one
CN102258000A (en) * 2011-04-11 2011-11-30 李翊玮 Safe and environmentally-friendly method for preventing and controlling cigarette beetle in cigarette factory
CN104430330A (en) * 2013-09-15 2015-03-25 苏州研迪智能科技有限公司 Lure core for prevention and control of cigarette beetles
CN105981722A (en) * 2015-03-04 2016-10-05 温州医科大学 Lasioderma serricorne (fabricius) sex pheromone and lure thereof
CN104914184A (en) * 2015-06-05 2015-09-16 广西中烟工业有限责任公司 Cold trap capturing-gas chromatography/mass spectrum combined detection method for furan in cigarette mainstream smoke
CN108353901A (en) * 2018-02-02 2018-08-03 武汉东昌仓贮技术有限公司 A kind of attractant and lure for luring control cigarette beetle

Non-Patent Citations (7)

* Cited by examiner, † Cited by third party
Title
ERASMUS CUDJOE 等: "Headspace gas chromatography-mass spectrometry a fast approach to the identification and determination of 2-alkyl-3- methoxypyrazinepheromones in ladybugs", 《ANALYST》 *
国家食品药品监督管理局药品审评中心: "《药品技术评价文集》", 31 December 2007, 中国医药科技出版社 *
尹炯 等: "固相微萃取-气相色谱-质谱联用法分析香蕉球茎象甲虫体挥发物", 《中国农学通报》 *
杜少芳 等: "梨小食心虫性诱芯中活性成分的气相色谱-质谱定量分析", 《山西农业科学》 *
毛若云 等: "烟草甲虫雌性信息素的合成及应用", 《中国烟草学报》 *
范晓军 等: "昆虫性信息素研究进展", 《安徽农业科学》 *
陈海滨 等: "烟草甲性信息素及其异构体的简易合成法", 《农药学学报》 *

Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN114062538A (en) * 2021-11-03 2022-02-18 莆田海关综合技术服务中心 Agilawood GC-MS fingerprint spectrum construction method
CN114062538B (en) * 2021-11-03 2024-05-10 莆田海关综合技术服务中心 Construction method of agilawood GC-MS fingerprint
CN114814021A (en) * 2022-04-21 2022-07-29 浙江省化工产品质量检验站有限公司 Detection method and application of sex pheromone pesticide of ostrinia furnacalis
CN114814021B (en) * 2022-04-21 2023-02-24 浙江省化工产品质量检验站有限公司 Detection method and application of sex pheromone pesticide of ostrinia furnacalis

Also Published As

Publication number Publication date
CN111398501B (en) 2022-08-30

Similar Documents

Publication Publication Date Title
CN102004132B (en) Method for measuring alkaloid in tobacco and tobacco product
Chen et al. Mainstream smoke chemical analyses for 2R4F Kentucky reference cigarette
CN105954402B (en) Gas-chromatography-flame ion/tandem mass spectrum detection method of alkaloid in a kind of cigarette mainstream flue gas
CN103134850A (en) Tea quality rapid detection apparatus and detection method based on characteristic fragrance
CN111398501B (en) Method for determining content of sex pheromone in tobacco beetle sex pheromone lure core
CN107490636B (en) Method for measuring 8 carbonyl compounds in mainstream smoke of heated non-combustible cigarette
CN107271584B (en) Method for trapping carbonyl compounds and tobacco-specific nitrosamines in cigarette mainstream smoke, extraction method and determination method
CN107561182A (en) Volatility and the detection method of semi-volatile organic compounds in cigarette mainstream flue gas
CN106932462A (en) A kind of method of quick measure Determination of Nicotine Content of Tobacco
CN103293267A (en) GC-MS/MS (gas chromatography-tandem mass spectrometry) method for analyzing pyrethroid pesticide residue in tobacco and tobacco product
CN102226786A (en) Method for accurately measuring free nicotine in main stream cigarette smoke
CN105823839B (en) Piece cigarette absorbs the evaluation method of feed liquid effect during a kind of leaves storage
CN112220095A (en) Cigarette production method based on temperature of moisture regain area and cigarette
CN111855866A (en) Method for rapidly determining formaldehyde in tobacco additive
CN105784886A (en) Gas chromatography-tandem mass spectrum detection method for hydrazine in cigarette mainstream smoke
CN109975443B (en) Method for detecting aldehydes in cigarette filter
CN110470768A (en) Pyrazosulfuron in a kind of measurement water quality, Hostathion, butachlor residue amount method
CN104897836B (en) The method of quinic acid, test kit and application thereof in detection sample
CN106442750B (en) A kind of method of free gossypol detoxification situation in evaluation cottonseed oil
CN104849391B (en) A kind of extract the method for chinic acid, kit and application thereof in sample
CN108088932A (en) A kind of ramuscule cigarette mainstream is by the computational methods of furans in mouth flue gas
CN114062537A (en) Method for accurately detecting diffusion rate of feed liquid applied in heated cigarette
CN108614060B (en) Method for measuring fluorochloropyridyl ester in rapeseeds by gas chromatography-mass spectrometry
CN113155931A (en) Method for detecting chloride ions in tobacco and tobacco planting soil
CN103115981B (en) Quantitative detection method for riboflavin in tobacco

Legal Events

Date Code Title Description
PB01 Publication
PB01 Publication
SE01 Entry into force of request for substantive examination
SE01 Entry into force of request for substantive examination
GR01 Patent grant
GR01 Patent grant