CN106706824A - Method for detecting insect in-vivo juvenile hormone JH II based on chromatography-mass spectrometry - Google Patents
Method for detecting insect in-vivo juvenile hormone JH II based on chromatography-mass spectrometry Download PDFInfo
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- CN106706824A CN106706824A CN201510783627.3A CN201510783627A CN106706824A CN 106706824 A CN106706824 A CN 106706824A CN 201510783627 A CN201510783627 A CN 201510783627A CN 106706824 A CN106706824 A CN 106706824A
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- acetonitrile
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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
- G01N30/88—Integrated analysis systems specially adapted therefor, not covered by a single one of the groups G01N30/04 - G01N30/86
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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
- G01N30/04—Preparation or injection of sample to be analysed
- G01N30/06—Preparation
Abstract
The invention discloses a method for detecting insect in-vivo juvenile hormone JH II based on chromatography-mass spectrometry and relates to application of analytical chemistry in entomology research. The method comprises the specific steps that an insect sample is taken, grinding balls, acetonitrile, a sodium chloride water solution and normal hexane are added for grinding, high-speed centrifugation is performed to obtain a normal-hexane-layer crude extract, then normal hexane is added to the sample for two times of grinding and extraction, the crude extract obtained through three times of grinding is added to a collecting bottle, and nitrogen blow-drying is performed; re-dissolution is performed with an acetonitrile-water solution, then the acetonitrile is eluted for three times by using a solid-phase extraction column, and eluant in a collecting box is taken out and subjected to nitrogen blow-drying; re-dissolution is performed with an acetonitrile-water solution, and analysis is performed by using a liquid chromatograph-mass spectrometer. The detecting method is high in sensitivity, strong in matrix interference resisting capability and good in repeatability and can provide help for research of in-vivo juvenile hormone JH II change laws of insects at all stages.
Description
Technical field
The invention belongs to analytical chemistry field, and in particular to one kind is based on juvenile hormone JH in insect bodies associated with liquid chromatography mass
The detection method of II, using extracting, purifying pretreatment process, liquid chromatogram is separated, the analysis of triple level Four bar Mass Spectrometer Methods
Learn the method that technological means is detected to the juvenile hormone JH II contents in insect bodies.
Background technology
Insect is animal most flouring in the world, and key player is played in biosphere.Study growth rhythm, the physiology of insect
Function, it is significant to control, management insect.Juvenile hormone is synthesized and is secreted into hemolymph by insect corporal allata
A kind of sesquiterpenoid.It can adjust many physiological functions of insect, including growth, breeding, polymorphism, diapause and generation
Pheromones etc..In view of extensive influence of the juvenile hormone on insect, sets up a kind of reliable and stable method for detecting juvenile hormone, can
Tool is provided with the research for insect.
Earliest juvenile hormone detection method is bioassary method, and juvenile hormone is extracted it makes use of the dermal cell for updating
Thing has hypersensitivity, and the activity to juvenile hormone in tissue block or hemolymph extract is detected.But the method is unable to area
Which kind of juvenile hormone is occurred that in decomposing biological sample, and is difficult the quantitative accuracy of control.Radioimmunoassays are using anti-
Body and 3 kinds of juvenile hormones produce specific combination, and the test of simplicity can be carried out to juvenile hormone.Distinguish different types of
, it is necessary to different antibody, this defect limits the use of radioimmunoassays to juvenile hormone.With chromatographic technique in recent years
Development, increasing scholar is detected using chromatographic technique to juvenile hormone.Gas chromatography combined with mass spectrometry technology can be to protecting
Young hormone carry out accurately it is qualitative, Bergot et al. reports that its Monitoring lower-cut has reached 1-2ng/g, however, this method need
Cumbersome pre-treatment step.Liquid chromatography mass GC-MS is quantitative using liquid phase separation, mass spectrometry, wherein, liquid chromatogram-
Triple level Four bar mass spectrometric hyphenated techniques, can be separated by liquid chromatogram, the mass spectrographic selection ion scan of two-stage, just for target
The daughter ion of juvenile hormone detected, matrix interference is excluded to greatest extent.It is mostly the report on detection JH III in document
Road, so far, there is not yet liquid-liquid extraction, SPE are combined to insect with liquid chromatogram-triple level Four bar combination mass-spectrometric techniques
The relevant report of internal juvenile hormone JH II detections.
The content of the invention
The present invention is for the juvenile hormone JH low technical deficiencies of II detection sensitivities in existing insect bodies, it is proposed that utilize liquid-liquid extraction
Purification, Solid phase extraction, the method for juvenile hormone JH II in liquid chromatogram separation and triple level Four bar Mass Spectrometer Method insect bodies,
The method can exclude the interference that other materials are detected to juvenile hormone JH II in insect bodies, high etc. with reproducible, sensitivity
Feature, it is adaptable to the detection of juvenile hormone JH II, research in insect bodies.
Technical scheme is as follows：
(1) insect sample 50-200mg is taken, after weighing, mill ball is put into, acetonitrile, the 2% of 250 μ L of 250 μ L is added
Sodium-chloride water solution and 500 μ L dissolve the n-hexane of 1ng/mL methoprenes, grind 2min, 12000g centrifugations 5min at 4 DEG C,
Supernatant n-hexane layer is extracted, adds the n-hexane of 500 μ L, milling and extracting supernatant to repeat once, crude extract is integrated with into receipts
Collection bottle, vortex 1min, low-speed centrifugal 2000g, nitrogen is slowly dried up, and obtains insect sample crude extract；Internal standard methoprene is whole
Variation tendency in experimentation to object juvenile hormone JH II is similar, can be good at monitoring guarantor in whole analyte detection process
The change of young hormone JH II, it is ensured that dosing accuracy of the whole detection method to juvenile hormone JH II.
(2) insect sample crude extract is redissolved with the aqueous solution of the 200 μ L containing 60% volumes of acetonitrile, then vortex 1min will redissolve
Liquid crosses solid-phase extraction column (wherein solid-phase extraction column uses the prewashing of 1mL methyl alcohol twice in advance), then is eluted 3 times with 200 μ L acetonitriles,
The eluent in disposable box is taken out, vortex 1min, low-speed centrifugal 2000g, nitrogen drying obtain insect sample extract；
(3) insect sample extract, vortex 1min, standby liquid chromatogram are redissolved with the aqueous solution of the 100 μ L containing 60% volumes of acetonitrile
GC-MS is analyzed.
Liquid chromatogram separation condition is：PFP chromatographic columns, specification be 100mm × 2mm × 1.7 μm, flow velocity 0.2mL/min,
45 DEG C of column temperature, sampling volume is 20 μ L.Liquid chromatogram mobile phase A phases are ammonium acetate containing 1mM, the water of 0.2% volumes of acetonitrile
Solution, B phases are the aqueous solution of 95% volumes of acetonitrile containing 1mM ammonium acetates, and using Gradient program, initial mobile phase is 40%B,
80%B linearly is raised in 8min, 100%, 10.1min is increased in subsequent 2min and is returned to 40%B and is balanced 5min.
Mass spectrum uses triple quadrupole rods tandem mass spectrometries, and Mass Spectrometer Method condition is：Using ESI sources positive ion mode, ion source interface
Voltage 4.0kV, atomization gas, dries gas and is all nitrogen, respectively 3L/min and 10L/min, and heating gas is air 10L/min,
Collision gas are argon gas, 250 DEG C of desolventizing pipe temperature, 400 DEG C of heating block temperature, and MRM acquisition parameters are, juvenile hormone JH
II quota ion pairs 281.1>294.35, impact energy -8V, qualitative ion pair 281.1>147.2, impact energy -13V, internal standard alkene worm
Ester quota ion pair 279.3>191.3, impact energy -11V, qualitative ion pair 279.3>237.3, impact energy -10V.
This method fully utilizes purifying technology-liquid-liquid extraction, the SPE of analytical chemistry, and employs high-efficient liquid phase color
Spectrum-triple quadrupole rods tandem mass spectrometry technologies, largely exclude what other materials in insect bodies were detected to juvenile hormone JH II
Interference, and instrumental sensitivity is high, test limit reaches 0.2pg.The internal standard methoprene of use swashs in whole extraction process with guarantor children
Plain JH II changes are consistent：Used as abscissa, the corresponding instrument of each concentration point rings each concentration point that juvenile hormone JH II are configured to
The ratio that should be responded with internal standard is as ordinate, linearly dependent coefficient R2>0.99；To adding basic, normal, high concentration in insect specimen
Juvenile hormone JH II, recovery of standard addition can reach 72.7%-87.4%.Document report only has Japanese Shiotsutki et al. uses and spreads out
Biochemical method detects JH II, and remaining is the method for detection JH III, and majority is then the sample introduction after purifying using just extraction.With
Existing method is compared, and this method pretreatment is simple, and sensitivity is high, and anti-matrix interference ability is strong, reproducible, can be insect
The research of juvenile hormone JH II Changing Patterns provides help in each period body.
Brief description of the drawings
Fig. 1 is the standard sample spectrogram of juvenile hormone JH II and internal standard methoprene；
Fig. 2 is the spectrogram that juvenile hormone JH II and internal standard methoprene are detected in insect specimen；
Fig. 3 juvenile hormone JH II linear standard curves.
Specific embodiment
Embodiment one is based on the evaluation of juvenile hormone JH II methods in liquid chromatography mass combination detection insect bodies
It is a series of solution of the dilution in acetonitrile of 1mg/mL juvenile hormone JH II standard specimens volumetric concentration 60% into various concentrations by concentration
(20ng/mL, 10ng/mL, 5ng/mL, 1ng/mL, 0.5ng/mL, 0.1ng/mL, 0.05ng/mL, 0.025ng/mL,
0.01ng/mL).Then 200 μ L various concentrations standard specimen solutions are taken respectively, and (concentration is 50 to add 20 μ L internal standard methoprenes solution
Ng/mL) mix, treat Instrumental Analysis.Liquid chromatography mass separation is carried out using the standard specimen solution of target various concentrations in above-mentioned addition
Analysis, investigates the linear of instrumental method, and it is bent to draw linear criterion with the relative area at the concentration of juvenile hormone JH II and peak as coordinate
Line, linearly dependent coefficient R2It is 0.9974 (Fig. 3), it is linear to meet analysis requirement.
By 8 parts of bollworm sample, mill ball, the acetonitrile of 250 μ L, 2% sodium-chloride water solution, 500 of 250 μ L are separately added into
The n-hexane of the μ L methoprenes of internal standard containing 1ng/mL, grinds 2min, and 12000g centrifugations 5min, extracts supernatant n-hexane at 4 DEG C
Layer, then to adding the pure hexane regrindings of 500 μ L in the residue extracted after supernatant, extracting supernatant, repeat grinding, extract
Twice (altogether extract three times), the hexane solution of crude extract must be contained by above-mentioned liquid-liquid extraction method, merge all 8 parts just oneself
Alkane solution is well mixed, and is then divided into 8 parts, every group 2 parts, totally 4 groups.1,2 part used as blank control group；3,4 parts
5pg standard specimens are added, as group 2；5,6 parts of addition 10pg standard specimens, as group 3；7,8 parts of addition 20pg standard specimens, as
Group 4.Again liquid chromatography mass point is carried out respectively through 200 μ L60% acetonitriles redissolution, SPE, the redissolution of 100 μ L60% acetonitriles
From analysis, recovery of standard addition is respectively 87.4%, 72.7% and 76.4%, and the rate of recovery meets analysis and requires.
Embodiment 24 age bollworm pattern detection
44, age bollworm samples are taken, is added in 2mL Eppendorf pipes, weigh to obtain quality 191.8mg, add grinding
Ball, adds acetonitrile, 2% sodium-chloride water solution of 250 μ L, the 500 μ L methoprenes of internal standard containing 1ng/mL of 250 μ L in order
N-hexane, grind 2min, 12000g centrifugations 5min at 4 DEG C extracts supernatant n-hexane layer, then to adding 500 in residue
Supernatant is extracted in the pure hexane of μ L, grinding, then is repeated to extract once with pure hexane, and crude extract is integrated with into 2mL Eppendorf
Pipe, vortex 1min, low-speed centrifugal 15s, nitrogen is slowly dried up, and obtains crude extract；To adding 200 μ L60% acetonitriles in crude extract
Redissolve, vortex 1min, liquid then will be redissolved after 1mL methyl alcohol prewashing solid-phase extraction column twice is used in advance, with 200 μ L acetonitriles
Wash-out 3 times, the eluent in disposable box is taken out, and rinses disposable box once with 200 μ L acetonitriles, and 2mL is entered together with eluent
Eppendorf is managed, low-speed centrifugal 15s, nitrogen drying, obtains extract；Finally, extract, whirlpool are redissolved with 100 μ L60% acetonitriles
Rotation 1min, loads sample injection bottles of the 1.5mL with bushing pipe, carries out liquid chromatography mass combined instrument analysis.
Chromatographic isolation uses PFP chromatographic columns, and specification is：100mm × 2mm × 1.7 μm, flow velocity 0.2mL/min, 45 DEG C of column temperature,
Sampling volume is ammonium acetate containing 1mM, 0.2% acetonitrile for 20 μ L, A phases, and B phases are ammonium acetate containing 1mM, 95% acetonitrile,
Mobile phase is initiated with 40%B, and 0-8min, 40%B-80%B, 8-10min, 80%B-100%B, 10.1min returns to 40%B,
Balance 5min.Mass Spectrometer Method uses ESI sources positive ion mode, and ion source interface voltage 4.0kV, atomization gas 3L/min do
Pathogenic dryness 10L/min, heats gas 10L/min, 250 DEG C of desolventizing pipe temperature, 400 DEG C of heating block temperature, MRM collection ginsengs
Number is, juvenile hormone JH II quota ion pairs 281.1>294.35, internal standard methoprene quota ion pair 279.3>191.3.
Using above-mentioned analysis method, the juvenile hormone JH II and the standard sample spectrogram of internal standard methoprene for obtaining are shown in Fig. 1, in insect
The juvenile hormone JH II and the spectrogram of internal standard methoprene detected in sample are shown in Fig. 2.Using inner mark method ration, in 4 age bollworms
The content about 0.17pg/mg of the juvenile hormone JH II detected in sample.
Embodiment 33 age bollworm pattern detection
36, age bollworm samples are taken, quality 127.2mg is weighed to obtain, mill ball, the acetonitrile of 250 μ L, the 2% of 250 μ L is added
The n-hexane of sodium-chloride water solution, the 500 μ L methoprenes of internal standard containing 1ng/mL, grinds 2min, 12000g centrifugations 5min at 4 DEG C,
Supernatant n-hexane layer is extracted, then repeats to extract twice with the pure hexanes of 500 μ L, crude extract is integrated with into 2mL Eppendorf
Pipe, vortex 1min, low-speed centrifugal 15s, nitrogen drying；200 μ L60% acetonitriles are added in crude extract after being dried up to nitrogen, is vortexed
1min, then liquid will be redissolved cross solid-phase extraction column and enter disposable box, eluted 3 times with 200 μ L acetonitriles, by the eluent in disposable box
Take out, and disposable box is rinsed once with 200 μ L acetonitriles, 2mL Eppendorf are entered together with eluent and is managed, low-speed centrifugal 15s,
Nitrogen is dried up；Extract is redissolved with 100 μ L60% acetonitriles, is vortexed, sample injection bottles of the 1.5mL with bushing pipe is moved into, through liquid chromatogram matter
The analysis of spectrum combined instrument and calculating, using inner mark method ration, the juvenile hormone JH II's detected in 3 age bollworm samples contains
Amount is about 0.10pg/mg.
Claims (9)
1. in a kind of insect bodies of application of gas chromatorgraphy/mass juvenile hormone JH II detection method, it is characterised in that including such as flow down
Journey step：
(1) insect sample 50-200mg is taken, mill ball is put into, the 5-20 times of second of (volume μ L/ sample quality mg) is added
Concentration 1ng/mL-10ng/mL methoprenes are dissolved with nitrile, sodium-chloride water solution and n-hexane, wherein n-hexane as internal standard,
N-hexane layer is extracted in grinding, centrifugation；
Extraction is ground to the n-hexane of the n-hexane layer same volume for repeating to add and extract in residue again, this process is repeated
1-3 times；
Receiving flask is incorporated to by the n-hexane of extraction is laminated, and nitrogen drying obtains insect sample crude extract；
(2) add 160-240 μ L acetonitrile-aqueous solutions to redissolve to insect sample crude extract, be vortexed, then will redissolve liquid and cross solid phase
Extraction column, is eluted 2-4 times with acetonitrile, takes out the eluent in disposable box, and nitrogen drying obtains insect sample extract；
(3) add 80-120 μ L to be redissolved containing acetonitrile-aqueous solution to insect sample extract, be vortexed, carry out liquid chromatography mass connection
Analyzed with instrument.
2. detection method according to claim 1, it is characterised in that：
The liquid chromatogram separation condition used in step (3) for：PFP chromatographic columns, specification is 100mm × 2mm × 1.7 μm,
Flow velocity 0.2mL/min, 45 DEG C of column temperature, sampling volume is 20 μ L；Liquid chromatogram mobile phase A phases be ammonium acetate containing 1mM,
The aqueous solution of 0.2% volumes of acetonitrile, B phases are ammonium acetate containing 1mM, the aqueous solution of 95% volumes of acetonitrile, using Gradient program, are risen
Beginning mobile phase is volumetric concentration 40%B, and linearly volumetric concentration 80%B is raised in 8min, is increased in subsequent 2min
100%B, 10.1min return to 40%B and balance 5min；
The mass spectrum used in step (3) is triple quadrupole rods tandem mass spectrometries, and Mass Spectrometer Method condition is：Using ESI sources cation mould
Formula, ion source interface voltage 4.0kV, dries gas and is all nitrogen, respectively 3L/min and 10L/min atomization gas, heats gas
It is air 10L/min, collision gas are argon gas, 250 DEG C of desolventizing pipe temperature, 400 DEG C of heating block temperature, MRM collection ginsengs
Number is, juvenile hormone JH II quota ion pairs 281.1>294.35, impact energy -8V, qualitative ion pair 281.1>147.2, collision
Can -13V, internal standard methoprene quota ion pair 279.3>191.3, impact energy -11V, qualitative ion pair 279.3>237.3, collision
Can -10V.
3. detection method according to claim 1, it is characterised in that：Sodium-chloride water solution sodium chloride-containing in step (1)
Concentration is 1%-5% (quality g/ volume mL), and the volume (μ L) of addition acetonitrile and the volume (μ L) of sodium-chloride water solution are same
It it is 5-10 times of insect sample quality (mg), the volume (μ L) for adding n-hexane is the acetonitrile and sodium-chloride water solution for adding
2-3 times of volume.
4. detection method according to claim 1, it is characterised in that：Grinding frequency 15-20 times is per second, when grinding every time
Between 2-3min.
5. detection method according to claim 1, it is characterised in that：160-240 μ L second is added to insect sample crude extract
The volume ratio of the nitrile-aqueous solution, wherein acetonitrile-aqueous solution be 5/4-5/2, with acetonitrile elute, every time wash-out acetonitrile content equivalent to
Cross the multiple liquor capacity of solid-phase extraction column 2-3 times.
6. detection method according to claim 1, it is characterised in that：Solid-phase extraction column requirement is filled with reverse phase filler
96 orifice plates, using 96 hole malleation extraction elements.
7. detection method according to claim 1, it is characterised in that：80-120 μ L are added to contain to insect sample extract
Acetonitrile-aqueous solution redissolves, wherein wherein the volume ratio of acetonitrile-aqueous solution is 5/4-5/2.
8. detection method according to claim 1, it is characterised in that：Juvenile hormone JH II use inner mark method ration, alkene
Worm ester is internal standard, is calculated according to linear quantitative curve.
9. detection method according to claim 1, it is characterised in that：Redissolve solid-phase extraction column before liquid crosses solid-phase extraction column
In advance with 1mL methyl alcohol prewashing 1-6 times.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108279273A (en) * | 2017-12-28 | 2018-07-13 | 常州胜杰化工有限公司 | A kind of HPLC analytical method of S- hydroprenes |
| CN114624365A (en) * | 2022-04-18 | 2022-06-14 | 中国测试技术研究院 | Method for simultaneously determining residues of three methoprene juvenile hormone analogues in tea |
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| CN104020223A (en) * | 2014-04-14 | 2014-09-03 | 常州胜杰化工有限公司 | Method for analyzing mass fraction of S-methoprene |
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| JPH04321641A (en) * | 1991-04-19 | 1992-11-11 | Mitsubishi Kasei Corp | Production of terpene alpha-ketols |
| WO2015132592A1 (en) * | 2014-03-06 | 2015-09-11 | Norbrook Laboratories Limited | Novel isoxazolines and their use in controlling pests |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108279273A (en) * | 2017-12-28 | 2018-07-13 | 常州胜杰化工有限公司 | A kind of HPLC analytical method of S- hydroprenes |
| CN114624365A (en) * | 2022-04-18 | 2022-06-14 | 中国测试技术研究院 | Method for simultaneously determining residues of three methoprene juvenile hormone analogues in tea |
| CN114624365B (en) * | 2022-04-18 | 2023-08-08 | 中国测试技术研究院 | Method for simultaneously determining residues of three methoprene juvenile hormone analogues in tea |
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