CN111323506A - Method for determining phytohormone in high-fat plant sample - Google Patents
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Abstract
The invention discloses a method for measuring phytohormone in a high-fat plant sample, which comprises a pretreatment process and a quantitative analysis process, wherein the pretreatment process comprises solvent extraction, solid-phase microextraction synchronous derivatization reaction and elution collection, and the method also comprises the step of carrying out the quantitative measurement of the phytohormone by a liquid chromatography-mass spectrometry analysis method; the method is realized by using a novel magnetic nano material Fe3O4/Ti3C2β -Cyclodextrin useful for plant stimulationThe method has the advantages of high selectivity, simple steps in the analysis and detection process, capability of realizing high-sensitivity and high-accuracy determination of the phytohormone in the high-oil plant sample, environmental friendliness, simplicity in operation, rapidness, high efficiency, sensitivity and the like.
Description
Technical Field
The invention relates to the field of chemical analysis, in particular to a method for determining phytohormone in a high-fat plant sample.
Background
Plant hormones are highly bioactive small signaling molecules that are involved in regulating plant growth and development and respond to external stimuli. It is known that hormones produced in plants mainly include auxins, Gibberellins (GA), cytokinins, abscisic acid (ABA), ethylene, brassinosteroids, etc., and how to directly and accurately measure the variety and concentration change of phytohormones is a key point of phytology research.
Rape, soybean, sunflower, peanut and cottonseed are five major oil crops in the world, and play a significant role in edible vegetable oil supply in China. The plant hormone has obvious influence on seed germination, seedling growth, yield traits and the like of oil crops such as rape, soybean, peanut and the like, but the quantitative determination of the plant hormone is difficult to perform due to the interference of the oil matrix in the high-oil plant sample, and the measurement accuracy is low. At present, the analysis of phytohormones in high-fat plant samples specifically faces three major problems: firstly, the concentration of the phytohormone in the plant body is low, and is only in ng/g or even pg/g grade; secondly, the matrix interference is large, the matrix in the plant body is complex, and the lipid interference of high-oil plant samples such as rape seeds is large; thirdly, the amount of plant samples is small, and with the deep research of the action mechanism of plant hormone molecules, the quantitative detection of tiny plant tissues or organs is needed. Therefore, the method has important research significance for carrying out high-sensitivity detection on the phytohormone in the trace plant sample.
Disclosure of Invention
The present invention is directed to solving at least one of the problems of the prior art. Therefore, the invention provides a method for measuring the phytohormone, which can detect the phytohormone in a high-fat plant sample with high sensitivity.
The method comprises a pretreatment process and a quantitative analysis process, wherein the pretreatment process comprises the following steps:
s1, extracting the treated plant sample by using a solvent to obtain a sample solution;
s2, adding a magnetic nano material and a derivatization reagent into the sample solution, carrying out solid phase microextraction synchronous derivatization reaction on the plant hormone in the sample solution, and then separating and collecting the magnetic nano material;
s3, eluting the magnetic nano material obtained in the step S2, and collecting supernatant;
wherein the magnetic nano material is Fe3O4/Ti3C2β -Cyclodextrin.
The method provided by the embodiment of the invention has at least the following beneficial effects: the method can realize high sensitivity and high accuracy determination of the phytohormone in the high-oil plant sample through the pretreatment steps of matrix dispersion, magnetic solid-phase microextraction synchronous derivatization and the like, has simple steps in the analysis and detection process, has no transfer in the whole pretreatment process, can reduce loss, and can detect the phytohormone in a trace sample; magnetic nanomaterial Fe used in the invention3O4/Ti3C2The first time the/β -cyclodextrin is based on Ti2C3The novel nano magnetic extraction adsorbent synthesized by modifying the material has high selectivity to phytohormone.
According to some embodiments of the invention, the magnetic nanomaterial is prepared by:
s01, etching Ti by using hydrofluoric acid solution3AlC2Reacting at the temperature of (25-35) DEG C for 20-30 h, washing and drying to obtain Ti3C2Powder;
s02, and Ti prepared in the step S013C2With Fe3O4Mixing, ultrasonic treating and drying to obtain Fe3O4/Ti3C2A complex;
s03, and Fe prepared in the step S023O4/Ti3C2Mixing with β -cyclodextrin, heating at 55-65 deg.C for 3-5 h, washing, and drying to obtain magnetic nanometer material Fe3O4/Ti3C2β -Cyclodextrin.
The invention discloses a magnetic dispersion solid phase microextraction technology, which is a rapid and efficient extraction mode generated by combining matrix dispersion and magnetic solid phase microextraction3O4/Ti3C2The/β -cyclodextrin is used as an adsorbent, high-efficiency extraction of different target phytohormones is realized through a high-selectivity adsorption material, and high-sensitivity analysis of the target is realized.
Preferably, the Ti is3C2With Fe3O4The mass ratio of (2-3): 1; said Fe3O4/Ti3C2The mass ratio of the cyclodextrin to the β -cyclodextrin is 1 (15-20).
According to some embodiments of the invention, the plant hormone comprises at least one of gibberellins, growth hormones, jasmonates, and abscisic acid plant hormones.
According to some embodiments of the present invention, the solvent of the solvent extraction in step S1 is at least one of lower alcohol, acetonitrile, chloroform, dichloromethane, ethyl acetate, acetone, and formic acid; preferably, the solvent is methanol. The extraction efficiency is high by using methanol as the solvent.
According to some embodiments of the present invention, the process of extracting the plant sample in step S1 further comprises adding a scavenger (florisil) and zirconium beads for shaking and crushing. The purifying agent and the zirconium beads are used for crushing the plant sample, and the matrix dispersion technology is used for reducing the interference of lipid and the like, so that the extraction efficiency of the phytohormone in the plant sample is improved.
Preferably, the extraction process in the step S1 includes the following specific steps of adding cold methanol into the plant sample, mixing by vortex for 30S, leaching at 4 ℃, centrifuging for 5min at 10000 × g at low temperature for 12h, and taking supernatant, wherein the temperature of the cold methanol is (-25-0) DEG C.
According to some embodiments of the invention, the derivatizing agent is EDC. The invention uses N-ethyl-N '- (3-dimethylaminopropyl) carbodiimide (N- (3-dimethyl-laminopropyl) -N' -ethyl carboxyl side, EDC) as a derivatization reagent for derivatization and mass spectrometry of auxin, jasmonic acid and abscisic acid plant hormone for the first time, and performs ammoniation reaction on carboxylic acid of the acid plant hormone in a water phase, thereby improving the mass spectrometry response of the acid plant hormone in a positive mode.
According to some embodiments of the invention, the solid-phase microextraction simultaneous derivatization reaction condition in step S2 is (35-45) ° c reaction (70-110) min. By optimizing the derivatization condition, the method has better derivatization reaction effect under the temperature and time of the optimized condition, and is favorable for complete derivatization reaction of the phytohormone in the plant sample.
Preferably, the solid-phase microextraction simultaneous derivatization reaction in step S2 specifically includes the following steps: adding 5mg of magnetic nano material, adding 50 mu L of 20mM EDC derivatization agent, carrying out water bath at 40 ℃, and synchronously finishing solid phase micro-extraction and derivatization.
According to some embodiments of the invention, the elution process in step S3 comprises the steps of: using ultrapure water solution, vortex analysis (15-25) min. The aqueous solution has the best elution effect.
According to some embodiments of the invention, the quantitative analysis process comprises the steps of: and (4) detecting the supernatant obtained in the step (3) by adopting a high performance liquid chromatography-mass spectrometry combined method, and calculating to obtain the concentration of the phytohormone.
According to some embodiments of the invention, the parameter conditions during the detection by the hplc-ms method are as follows:
liquid chromatography conditions: the mobile phase A is 0.1 percent of formic acid water solution, the mobile phase B is acetonitrile, and the mobile phase B is subjected to gradient elution from 10 percent to 40 percent;
mass spectrum conditions: the temperature of atomizing gas is 300 ℃; flow rate of atomizing gas: 8 mL/min-1(ii) a Atomizer pressure 30 psi; an ion source: 70 eV; the scanning mode is as follows: and (4) detecting multiple reactions.
By optimizing the conditions of the liquid mass spectrum, an accurate phytohormone detection result can be obtained.
Additional aspects and advantages of the invention will be set forth in part in the description which follows and, in part, will be obvious from the description, or may be learned by practice of the invention.
Drawings
FIG. 1 is a test chart of the magnetic nanomaterial of example 1 of the present invention, in which (a) and (b) are Ti, respectively3C2And Fe3O4/Ti3C2(iii) scanning Electron microscopy of/β -Cyclodextrin, (c) and (d) are respectively Ti3C2And Fe3O4/Ti3C2(iii) TEM image of/β -Cyclodextrin, (e) and (f) are Fe3O4/Ti3C2A scanning electron microscopy energy spectrum analysis chart of/β -cyclodextrin;
FIG. 2 is a schematic view of the measurement method in example 2 of the present invention;
FIG. 3 shows a standard solution (100. mu. g L) of 12 phytohormones in example 2 of the present invention-1) Multiple Reaction Monitoring (MRM) chromatograms.
Detailed Description
In order to explain technical contents, achieved objects, and effects of the present invention in detail, the following description is made with reference to the accompanying drawings in combination with the embodiments.
The materials and equipment used in the following examples are commercially available.
1、Ti3C2preparation of
10g of Ti were weighed3AlC2Adding 100mL of 40% hydrofluoric acid solution into the powder, magnetically stirring at 30 ℃ for 24h, and etching Ti3AlC2Al in the Al alloy to prepare two-dimensional layered Ti3C2Centrifuging, washing the obtained suspension with deionized water repeatedly, washing with ethanol for 3 times until pH reaches neutral, vacuum drying at 80 deg.C, and preparing to obtain Ti3C2And (3) powder.
2、Fe3O4/Ti3C2Preparation of the Complex
100mg of Ti3C2And 40mg of Fe3O4The nanoparticles were dispersed in 80mL and 20mL deionized water with sonication for 30min, respectively. And carrying out ultrasonic treatment for 6h after mixing. Filtering to obtain Fe3O4/Ti3C2And drying the prepared composite in a vacuum drying oven at 80 ℃ for 24 hours.
3、Fe3O4/Ti3C2Preparation of/β -Cyclodextrin
100mg Fe3O4/Ti3C2And 2g of β -cyclodextrin dispersed in 60mL of deoxygenated water and stirred for 20min, oil bath at 60 ℃ for 4h3O4/Ti3C2And/β -cyclodextrin is repeatedly leached and vacuum-dried at 50 ℃ for 24 h.
FIG. 1 is an electron microscope image of the magnetic nanomaterial, wherein Ti is shown in FIG. 1(a) and Ti is shown in FIG. 1(b), respectively3C2And Fe3O4/Ti3C2[ scanning Electron microscopy ] of/β -Cyclodextrin, FIG. 1(c) and FIG. 1(d) are each Ti3C2And Fe3O4/Ti3C2(iii) TEM images of/β -Cyclodextrin, (e) and (f) are Fe3O4/Ti3C2(iii) SEM energy spectrum analysis of/β -Cyclodextrin As shown in FIGS. 1(a) and 1(c), Ti3C2Is a two-dimensional layered structure; (b) the electron micrograph of (d) shows Fe prepared3O4And β -cyclodextrin are uniformly loaded on Ti3C2The above. The energy spectrum analysis charts of FIG. 1(e) and FIG. 1(f) confirm that the magnetic nano-material contains Ti and Fe elements.
1. matrix dispersion degreasing: taking a single fresh rape seed (5-8mg), adding 2mg of purifying agent and a single zirconium bead, shaking and grinding for 4min, adding phytohormone internal standard (see table 2 in detail) into the uniformly ground sample, swirling for 30s, and standing for 10 min.
2. And (3) extraction: adding 200 μ L cold methanol, high speed vortex mixing, standing at 4 deg.C overnight for leaching for 12h, centrifuging at 10000rpm for 5min, and collecting the upper layer extractive solution.
3. Magnetic solid phase microextraction synchronous derivatization: 5mg of magnetic nanomaterial (Fe) was added3O4/Ti3C2/β -Cyclodextrin), 50. mu.L of 20mM EDC was added, the mixture was shaken in a water bath at 40 ℃ for 90min, magnetic separation was carried out, the supernatant was discarded, 50. mu.L of ultrapure water was added for elution, and the supernatant was vortexed for 20min and transferred to a vial with an insert tube.
4. And (3) putting the sample feeding bottle into a high performance liquid chromatography-mass spectrometry combined instrument for detection, calculating the concentration of the target object before and after extraction, wherein the chromatographic conditions and mass spectrometry conditions of phytohormone analysis are as follows:
4.1 chromatographic conditions
Chromatographic column Waters ACQUITY UPLC HSS T3100 mm × 2.1.1 μm;
column temperature: 40 ℃;
sample introduction amount: 10 mu L of the solution;
mobile phase: a: 0.1% aqueous formic acid; b: acetonitrile, gradient elution according to the following table;
table 1: gradient elution condition of liquid chromatogram mobile phase
4.2 Mass Spectrometry conditions
Liquid chromatogram-mass spectrum coupling interface: electrospray ionization (ESI) positive mode;
temperature of atomized gas: 300 ℃;
flow rate of atomizing gas: 8 mL/min-1；
Atomizer pressure: 30 psi;
ion source (EI): 70 eV;
the scanning mode is as follows: multiplex reaction detection (MRM);
table 2: mass spectrometric parameters of phytohormone derivatives to be analyzed
The above compound names and abbreviations are respectively: gibberellin (abbreviated GA) stands for gibberellins, Indole-3-acetic Acid (abbreviated IAA) for indoleacetic Acid, Aabbsciic Acid (abbreviated ABA) for abscisic Acid, and Jasmic Acid (abbreviated JA) for Jasmonic Acid.
5. And (3) measuring results: measurement of phytohormones in fresh rape seeds, 12 hormones in rape seeds were detected, and the results are shown in table 3 (below*RSD relative standard deviation (%):
table 3: 12 phytohormones and test data of standard recovery rate thereof
The recovery rate of the method is between 80.4 and 115.1 percent (see table 3), the Relative Standard Deviation (RSD) is 1.1 to 15.1 percent, and the linear correlation coefficient R is2>0.9928, the detection limit of the method is 0.002-0.23 ng/ml. The method synthesizes a novel magnetic nano material, combines the matrix dispersing and degreasing, the magnetic solid phase micro-extraction and the synchronous derivatization technology, has good detection limit and recovery rate, is sensitive and efficient, can accurately measure various plant hormone substances, and has important application value in the detection of the plant hormone in high-fat plant samples.
In the experimental process, the best experimental effect is obtained by optimizing experimental factors of all links, such as preparation of magnetic nano materials, dosage of adsorbent materials used for magnetic solid-phase microextraction, pH of a system, synchronous derivatization time of solid-phase microextraction, eluent and the like.
In conclusion, the beneficial effects of the invention are as follows:
(1) the invention is based on Ti for the first time2C3Material, modifying it and synthesizing a new-type magnetic nano material Fe3O4/Ti2C3β -cyclodextrin to achieve high selective extraction of phytohormones;
(2) the invention combines matrix dispersion degreasing, magnetic solid phase micro-extraction and derivatization to realize synchronous extraction and derivatization, and realizes high-sensitivity qualitative and quantitative analysis of the phytohormone in the multi-lipid sample by taking a liquid chromatography-mass spectrometry technology as a basic means;
(3) the method has the advantages of simple analysis and detection steps, no transfer in the whole pretreatment process, loss reduction, capability of detecting 5mg trace plant samples and realization of analysis and test of the phytohormones in the trace plant samples.
The foregoing is merely a preferred embodiment of the invention and is not intended to limit the invention in any manner. Although the present invention has been described with reference to the preferred embodiments, it is not intended to be limited thereto. Many possible variations and modifications may be made to the disclosed methods and techniques, or equivalents may be substituted for those skilled in the art without departing from the spirit and scope of the invention. Therefore, any simple modification, equivalent replacement, equivalent change and modification of the above embodiments according to the technical essence of the present invention are within the protection scope of the technical solution of the present invention.
Claims (10)
1. A method for measuring phytohormone in a high-fat plant sample is characterized by comprising a pretreatment process and a quantitative analysis process, wherein the pretreatment process comprises the following steps:
s1, extracting the plant sample by using a solvent to obtain a sample solution;
s2, adding a magnetic nano material and a derivatization reagent into the sample solution, carrying out solid phase microextraction synchronous derivatization reaction on the plant hormone in the sample solution, and then separating and collecting the magnetic nano material;
s3, eluting the magnetic nano material obtained in the step S2, and collecting supernatant;
wherein the magnetic nano material is Fe3O4/Ti3C2β -Cyclodextrin.
2. The method of claim 1, wherein the magnetic nanomaterial is prepared by:
s01, etching Ti by using hydrofluoric acid solution3AlC2Reacting at the temperature of (25-35) DEG C for 20-30 h, washing and drying to obtain Ti3C2Powder;
s02, and Ti prepared in the step S013C2With Fe3O4Mixing, ultrasonic treating and drying to obtain Fe3O4/Ti3C2A complex;
s03, and Fe prepared in the step S023O4/Ti3C2Mixing with β -cyclodextrin, heating at 55-65 deg.C for 3-5 h, washing, and drying to obtain magnetic nanometer material Fe3O4/Ti3C2β -Cyclodextrin.
3. The method of claim 1, wherein the plant hormone comprises at least one of gibberellins, growth hormones, jasmonates, and abscisic acid plant hormones.
4. The method of claim 1, wherein the solvent in step S1 is at least one of lower alcohol, acetonitrile, chloroform, dichloromethane, ethyl acetate, acetone, and formic acid; preferably, the solvent is methanol.
5. The method of claim 1, wherein the step of extracting the plant sample in step S1 further comprises adding a detergent and zirconium beads for shaking and crushing.
6. The method of claim 1, wherein the derivatizing agent is EDC.
7. The method of claim 1, wherein the solid-phase microextraction simultaneous derivatization reaction condition in step S2 is (35-45) ° c reaction (70-110) min.
8. The method of claim 1, wherein the elution process in step S3 comprises the steps of: vortex analysis (15-25) min using ultrapure water.
9. The method of claim 1, wherein the quantitative analysis process comprises the steps of: and (5) detecting the supernatant obtained in the step (S3) by adopting a high performance liquid chromatography-mass spectrometry combined method, and calculating to obtain the concentration of the phytohormone.
10. The method of claim 9, wherein the parameter conditions during the detection by the HPLC-MS method are as follows:
liquid chromatography conditions: the mobile phase A is 0.1 percent of formic acid water solution, the mobile phase B is acetonitrile, and the mobile phase B is subjected to gradient elution from 10 percent to 40 percent;
mass spectrum conditions: the temperature of atomizing gas is 300 ℃; flow rate of atomizing gas: 8 mL/min-1(ii) a Atomizer pressure 30 psi; an ion source: 70 eV; the scanning mode is as follows: and (4) detecting multiple reactions.
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