CN104820034A - Method for simultaneously determining multiple plant growth regulators in exported vegetables - Google Patents
Method for simultaneously determining multiple plant growth regulators in exported vegetables Download PDFInfo
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- CN104820034A CN104820034A CN201510238783.1A CN201510238783A CN104820034A CN 104820034 A CN104820034 A CN 104820034A CN 201510238783 A CN201510238783 A CN 201510238783A CN 104820034 A CN104820034 A CN 104820034A
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- 235000013311 vegetables Nutrition 0.000 title claims abstract description 30
- 239000005648 plant growth regulator Substances 0.000 title claims abstract description 26
- 238000000034 method Methods 0.000 title abstract description 28
- 239000007788 liquid Substances 0.000 claims abstract description 28
- 150000002500 ions Chemical class 0.000 claims description 43
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 claims description 24
- WEVYAHXRMPXWCK-UHFFFAOYSA-N Acetonitrile Chemical compound CC#N WEVYAHXRMPXWCK-UHFFFAOYSA-N 0.000 claims description 24
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 claims description 10
- 239000000126 substance Substances 0.000 claims description 9
- 239000006228 supernatant Substances 0.000 claims description 9
- 239000000243 solution Substances 0.000 claims description 8
- 230000014759 maintenance of location Effects 0.000 claims description 7
- 238000004949 mass spectrometry Methods 0.000 claims description 7
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 6
- 239000003630 growth substance Substances 0.000 claims description 6
- 238000002156 mixing Methods 0.000 claims description 6
- 230000010355 oscillation Effects 0.000 claims description 6
- 238000010998 test method Methods 0.000 claims description 6
- 150000001875 compounds Chemical class 0.000 claims description 5
- 239000011780 sodium chloride Substances 0.000 claims description 5
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- USFZMSVCRYTOJT-UHFFFAOYSA-N Ammonium acetate Chemical compound N.CC(O)=O USFZMSVCRYTOJT-UHFFFAOYSA-N 0.000 claims description 3
- 239000005695 Ammonium acetate Substances 0.000 claims description 3
- CSNNHWWHGAXBCP-UHFFFAOYSA-L Magnesium sulfate Chemical compound [Mg+2].[O-][S+2]([O-])([O-])[O-] CSNNHWWHGAXBCP-UHFFFAOYSA-L 0.000 claims description 3
- 229940043376 ammonium acetate Drugs 0.000 claims description 3
- 235000019257 ammonium acetate Nutrition 0.000 claims description 3
- 239000000872 buffer Substances 0.000 claims description 3
- 238000004364 calculation method Methods 0.000 claims description 3
- 238000011208 chromatographic data Methods 0.000 claims description 3
- 238000010828 elution Methods 0.000 claims description 3
- YTJSFYQNRXLOIC-UHFFFAOYSA-N octadecylsilane Chemical compound CCCCCCCCCCCCCCCCCC[SiH3] YTJSFYQNRXLOIC-UHFFFAOYSA-N 0.000 claims description 3
- 238000003825 pressing Methods 0.000 claims description 3
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- 238000005374 membrane filtration Methods 0.000 claims description 2
- OAKJQQAXSVQMHS-UHFFFAOYSA-N Hydrazine Chemical compound NN OAKJQQAXSVQMHS-UHFFFAOYSA-N 0.000 abstract description 47
- JLIDBLDQVAYHNE-YKALOCIXSA-N (+)-Abscisic acid Chemical compound OC(=O)/C=C(/C)\C=C\[C@@]1(O)C(C)=CC(=O)CC1(C)C JLIDBLDQVAYHNE-YKALOCIXSA-N 0.000 abstract description 6
- JTEDVYBZBROSJT-UHFFFAOYSA-N indole-3-butyric acid Chemical compound C1=CC=C2C(CCCC(=O)O)=CNC2=C1 JTEDVYBZBROSJT-UHFFFAOYSA-N 0.000 abstract description 5
- 230000008901 benefit Effects 0.000 abstract description 4
- SODPIMGUZLOIPE-UHFFFAOYSA-N (4-chlorophenoxy)acetic acid Chemical compound OC(=O)COC1=CC=C(Cl)C=C1 SODPIMGUZLOIPE-UHFFFAOYSA-N 0.000 abstract description 3
- RMOGWMIKYWRTKW-UONOGXRCSA-N (S,S)-paclobutrazol Chemical compound C([C@@H]([C@@H](O)C(C)(C)C)N1N=CN=C1)C1=CC=C(Cl)C=C1 RMOGWMIKYWRTKW-UONOGXRCSA-N 0.000 abstract description 3
- 239000005660 Abamectin Substances 0.000 abstract description 3
- OORIKNJWZHTXDC-UHFFFAOYSA-N CCCC(CC)C(CC)(C(=O)OCC)N Chemical compound CCCC(CC)C(CC)(C(=O)OCC)N OORIKNJWZHTXDC-UHFFFAOYSA-N 0.000 abstract description 3
- 239000005979 Forchlorfenuron Substances 0.000 abstract description 3
- 229930191978 Gibberellin Natural products 0.000 abstract description 3
- NWBJYWHLCVSVIJ-UHFFFAOYSA-N N-benzyladenine Chemical compound N=1C=NC=2NC=NC=2C=1NCC1=CC=CC=C1 NWBJYWHLCVSVIJ-UHFFFAOYSA-N 0.000 abstract description 3
- 239000005985 Paclobutrazol Substances 0.000 abstract description 3
- HFCYZXMHUIHAQI-UHFFFAOYSA-N Thidiazuron Chemical compound C=1C=CC=CC=1NC(=O)NC1=CN=NS1 HFCYZXMHUIHAQI-UHFFFAOYSA-N 0.000 abstract description 3
- MXWJVTOOROXGIU-UHFFFAOYSA-N atrazine Chemical compound CCNC1=NC(Cl)=NC(NC(C)C)=N1 MXWJVTOOROXGIU-UHFFFAOYSA-N 0.000 abstract description 3
- FCRACOPGPMPSHN-UHFFFAOYSA-N desoxyabscisic acid Natural products OC(=O)C=C(C)C=CC1C(C)=CC(=O)CC1(C)C FCRACOPGPMPSHN-UHFFFAOYSA-N 0.000 abstract description 3
- GPXLRLUVLMHHIK-UHFFFAOYSA-N forchlorfenuron Chemical compound C1=NC(Cl)=CC(NC(=O)NC=2C=CC=CC=2)=C1 GPXLRLUVLMHHIK-UHFFFAOYSA-N 0.000 abstract description 3
- IXORZMNAPKEEDV-UHFFFAOYSA-N gibberellic acid GA3 Natural products OC(=O)C1C2(C3)CC(=C)C3(O)CCC2C2(C=CC3O)C1C3(C)C(=O)O2 IXORZMNAPKEEDV-UHFFFAOYSA-N 0.000 abstract description 3
- 239000003448 gibberellin Substances 0.000 abstract description 3
- ODCWYMIRDDJXKW-UHFFFAOYSA-N simazine Chemical compound CCNC1=NC(Cl)=NC(NCC)=N1 ODCWYMIRDDJXKW-UHFFFAOYSA-N 0.000 abstract description 3
- OVSKIKFHRZPJSS-UHFFFAOYSA-N 2,4-D Chemical compound OC(=O)COC1=CC=C(Cl)C=C1Cl OVSKIKFHRZPJSS-UHFFFAOYSA-N 0.000 abstract description 2
- 238000000746 purification Methods 0.000 abstract description 2
- YNWVFADWVLCOPU-MDWZMJQESA-N (1E)-1-(4-chlorophenyl)-4,4-dimethyl-2-(1H-1,2,4-triazol-1-yl)pent-1-en-3-ol Chemical compound C1=NC=NN1/C(C(O)C(C)(C)C)=C/C1=CC=C(Cl)C=C1 YNWVFADWVLCOPU-MDWZMJQESA-N 0.000 abstract 1
- DARPYRSDRJYGIF-PTNGSMBKSA-N (Z)-3-ethoxy-2-naphthalen-2-ylsulfonylprop-2-enenitrile Chemical compound C1=CC=CC2=CC(S(=O)(=O)C(\C#N)=C/OCC)=CC=C21 DARPYRSDRJYGIF-PTNGSMBKSA-N 0.000 abstract 1
- ZBIULCVFFJJYTN-UHFFFAOYSA-N 2-(4-fluorophenoxy)acetic acid Chemical compound OC(=O)COC1=CC=C(F)C=C1 ZBIULCVFFJJYTN-UHFFFAOYSA-N 0.000 abstract 1
- PWVXXGRKLHYWKM-UHFFFAOYSA-N 5-[2-(benzenesulfonyl)ethyl]-3-[(1-methylpyrrolidin-2-yl)methyl]-1h-indole Chemical compound CN1CCCC1CC(C1=C2)=CNC1=CC=C2CCS(=O)(=O)C1=CC=CC=C1 PWVXXGRKLHYWKM-UHFFFAOYSA-N 0.000 abstract 1
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- 229950008167 abamectin Drugs 0.000 abstract 1
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- YNWVFADWVLCOPU-MAUPQMMJSA-N uniconazole P Chemical compound C1=NC=NN1/C([C@@H](O)C(C)(C)C)=C/C1=CC=C(Cl)C=C1 YNWVFADWVLCOPU-MAUPQMMJSA-N 0.000 description 2
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- Other Investigation Or Analysis Of Materials By Electrical Means (AREA)
Abstract
The invention discloses a method for simultaneously determining multiple plant growth regulators in exported vegetables. The method comprises the following steps: extraction, purification, concentration, ultrahigh-performance liquid chromatography-triple quadrupole/composite linear ion hydrazine mass spectrometer (UHPLC-QTRAP) determination and the like. The method can simultaneously determine the 17 plant growth regulators, including gibberellin, indolyl-3-butyric acid, p-chlorophenoxyacetic acid, abamectin, diethyl aminoethyl hexanoate, atrazine, simazine, 6-benzyl aminopurine, 2,4-dichlorphenoxyacetic acid, forchlorfenuron, mepiquat chloride, chlormequat chloride, paclobutrazol, uniconazole, abscisic acid, thidiazuron and p-fluorophenoxyacetic acid. The method disclosed by the invention has the advantages of simple steps, short time consumption, high accuracy and high precision.
Description
Technical field
The invention belongs to chemical analysis detection field, be specifically related to the Simultaneously test method of 17 plant growth regulators in a kind of export vegetable.
Background technology
Vegetables are not only the main supply source of the mineral matter such as multivitamin and potassium, magnesium, calcium, phosphorus, iron and dietary fiber, and be the important sources of plant chemical ingredient as the antioxidant such as carotenoid, plant polyphenol, to Antioxidative Defense System in reinforcement and nutrition revision points, correct gene weakness and play an important role.In order to change the natural mode of vegetable growth, growth by chemical regulation, effectively improve Vegetable produce situation, improve vegetable yields and quality, plant growth regulator has been widely used in Vegetable produce.In recent years, the widespread use of plant growth regulator on vegetables, brings certain economic benefit to user.Such as, but the plant growth regulator of Residues in Vegetables brings potential safety hazard, reproduction and endocrine system disorder, immune dysfunction, cancer and other potential diseases equally also to the health of people.So while both needing to ensure agriculture economic interests; need again the healthy of Protection of consumer; what remain plant growth regulator in vegetables is detected as in order to a necessary job, not only contributes to supervision food security and also can use plant growth regulator and provide certain foundation.
At present, the detection method that domestic and international concerned plant growth regulator is residual mainly contains euzymelinked immunosorbent assay (ELISA) (ELISA), the chromatography of ions (IC), vapor-phase chromatography (GC), gas chromatography-mass spectrography (GC-MS), high performance liquid chromatography (HPLC) and Liquid Chromatography-Tandem Mass Spectrometry (LC-MS/MS).ELISA is adopted easily to produce false positive, use the complex operations usually will carrying out derivatization during GC and GC-MS, the sensitivity of HPLC is lower and be difficult to realize confirmatory analysis, and Liquid Chromatography-Tandem Mass Spectrometry (LC-MS/MS) can carry out qualitative and quantitative analysis to polycomponent simultaneously, and there is the advantages such as specificity is strong, selectivity good, sensitivity is high, compensate for the deficiency of preceding method, a series of advantages that LC-MS/MS possesses, determine its application prospect widely.
Summary of the invention
Given this, the object of this invention is to provide the Simultaneously test method of various plants growth regulator in a kind of export vegetable, employing UHPLC-QTRAP can detect 17 plant growth regulators in vegetables to be measured simultaneously, comprise gibberellin, indole-3-butyric acid, p-chlorophenoxyacetic acid, Avermectin, diethyl aminoethyl hexanoate, atrazine, Simanex, 6-benzyl aminopurine, 2,4-dichlorphenoxyacetic acids, forchlorfenuron, help strong element, cycocel, paclobutrazol, uniconazole P, abscisic acid, Thidiazuron, to fluorobenzene fluoroacetic acid.UHPLC-QTRAP had both retained the good selectivity of LC-MS/MS and sensitivity, also can be used as linear ion hydrazine and strengthened secondary fragment ion qualitative function.
The inventive method specifically comprises the steps:
1) extract
Add vegetables homogenate and contain the acetonitrile solution of 1% (v/v) acetic acid in centrifuge tube, the ratio of the acetonitrile solution of 1% (v/v) acetic acid is contained in the homogenate of every 1g vegetables and 2mL, horizontal oscillations 10min, the ratio adding 0.5g sodium chloride in the homogenate of every 1g vegetables again adds sodium chloride in centrifuge tube, vortex mixing 1min again, the centrifugal 3min of 5000r/min, Aspirate supernatant I is in centrifuge tube, to be clean;
2) sample is purified
Be equipped with in the centrifuge tube of supernatant I described in octadecylsilane chemically bonded silica and anhydrous magnesium sulfate being added by weight 1:5, the centrifugal 3min of vortex mixing 2min, 5000r/min, Aspirate supernatant II steams in bottle in revolving;
3) concentrated
To revolve steaming bottle and be placed in less than 40 DEG C water-bath concentrated by rotary evaporations to clean dry, add the acetonitrile of 1mL containing 1% (v/v) acetic acid, vortex oscillation, dissolving is revolved and is steamed residue in bottle, after membrane filtration, measures for UHPLC-QTRAP;
4) UPLC-MS/MS measures, and condition determination is as follows:
Chromatographic column: C18;
Mobile phase: acetonitrile-2mmol/L ammonium acetate buffer, gradient elution;
The reference retention time of each compound and mass spectrometry parameters, in table 1, are wherein with * to represent qualitative ion and quota ion;
Column temperature: 40 DEG C;
Flow velocity: 0.3mL/min;
Sample size: 10 μ L;
Prerun time: 1.0min;
Positive ion mode total run time: 5min;
Negative ion mode total run time: 6min;
Obtain UHPLC-QTRAP figure;
The reference retention time of table 1 17 plant growth regulators and mass spectrometry parameters
5) result calculates
With chromatographic data processor or the content pressing plant growth regulator in formula (1) calculating sample, result of calculation must deduct blank value;
In formula:
X
i---the content of test substance in sample to be tested, unit is milligrams per kilogram;
C
i---from the solution concentration of the test substance that UHPLC-QTRAP figure obtains, unit is micrograms per millilitre;
V---the final constant volume of sample liquid, unit is milliliter;
M---final sample to be tested quality representated by sample liquid, unit is gram.
In existing vegetable plant growth regulator detection method, do not adopt UHPLC-QTRAP to detect the method for 17 plant growth regulators simultaneously, conventional plant growth regulator detection side rule is employing high performance liquid chromatography, high-efficient liquid is in series mass spectroscopy and Ultra Performance Liquid Chromatography tandem mass spectrometry etc., as document " HPLC method and HPLC-MS/MS method detect plant growth promoter in fruits and vegetables and remain " and " Ultra Performance Liquid Chromatography-tandem mass spectrometry measures 6 plant growth regulators in Cereals and remains ".QTRAP had both retained the series connection good selectivity of level Four bar and sensitivity, also can be used as linear ion hydrazine and strengthened secondary fragment ion qualitative function." bar-hydrazine scanning " pattern, single injected sampling can obtain for quantitative MRM chromatogram and for two-stage system spectrogram qualitatively, compared with common triple level Four bar scan patterns, enhance secondary fragment ion scan, greatly improve the scan capability of MS/MS, be more conducive to the qualitative ability strengthening micro-target compound in complex dielectrics.The present invention can detect 17 plant growth regulators in export vegetable simultaneously, detecting step is easy, short, accuracy consuming time and precision high.
Accompanying drawing explanation
Fig. 1 is Ultra Performance Liquid Chromatography-triple level Four bar/compounded linear ion hydrazine mass spectrogram (0.1mg/L) of the gibberellin standard solution adopting the inventive method to obtain;
Fig. 2 is Ultra Performance Liquid Chromatography-triple level Four bar/compounded linear ion hydrazine mass spectrogram (0.1mg/L) of the indole-3-butyric acid standard solution adopting the inventive method to obtain;
Fig. 3 is Ultra Performance Liquid Chromatography-triple level Four bar/compounded linear ion hydrazine mass spectrogram (0.1mg/L) of the p-chlorophenoxyacetic acid standard solution adopting the inventive method to obtain;
Fig. 4 is Ultra Performance Liquid Chromatography-triple level Four bar/compounded linear ion hydrazine mass spectrogram (0.1mg/L) of the Avermectin standard solution adopting the inventive method to obtain;
Fig. 5 is Ultra Performance Liquid Chromatography-triple level Four bar/compounded linear ion hydrazine mass spectrogram (0.1mg/L) of the diethyl aminoethyl hexanoate standard solution adopting the inventive method to obtain;
Fig. 6 is Ultra Performance Liquid Chromatography-triple level Four bar/compounded linear ion hydrazine mass spectrogram (0.1mg/L) of the atrazine standard solution adopting the inventive method to obtain;
Fig. 7 is Ultra Performance Liquid Chromatography-triple level Four bar/compounded linear ion hydrazine mass spectrogram (0.1mg/L) of the Simanex standard solution adopting the inventive method to obtain;
Fig. 8 is Ultra Performance Liquid Chromatography-triple level Four bar/compounded linear ion hydrazine mass spectrogram (0.1mg/L) of the 6-benzyl aminopurine standard solution adopting the inventive method to obtain;
Fig. 9 is Ultra Performance Liquid Chromatography-triple level Four bar/compounded linear ion hydrazine mass spectrogram (0.1mg/L) of 2, the 4-dichlorphenoxyacetic acid standard solution adopting the inventive method to obtain;
Figure 10 is Ultra Performance Liquid Chromatography-triple level Four bar/compounded linear ion hydrazine mass spectrogram (0.1mg/L) of the forchlorfenuron standard solution adopting the inventive method to obtain;
Figure 11 be adopt the inventive method obtain help the Ultra Performance Liquid Chromatography of strong plain standard solution-triple level Four bar/compounded linear ion hydrazine mass spectrogram (0.1mg/L);
Figure 12 is Ultra Performance Liquid Chromatography-triple level Four bar/compounded linear ion hydrazine mass spectrogram (0.1mg/L) of the cycocel standard solution adopting the inventive method to obtain;
Figure 13 is Ultra Performance Liquid Chromatography-triple level Four bar/compounded linear ion hydrazine mass spectrogram (0.1mg/L) of the paclobutrazol standard solution adopting the inventive method to obtain;
Figure 14 is Ultra Performance Liquid Chromatography-triple level Four bar/compounded linear ion hydrazine mass spectrogram (0.1mg/L) of the uniconazole P standard solution adopting the inventive method to obtain;
Figure 15 is Ultra Performance Liquid Chromatography-triple level Four bar/compounded linear ion hydrazine mass spectrogram (0.1mg/L) of the abscisic acid standard solution adopting the inventive method to obtain;
Figure 16 is Ultra Performance Liquid Chromatography-triple level Four bar/compounded linear ion hydrazine mass spectrogram (0.1mg/L) of the Thidiazuron standard solution adopting the inventive method to obtain;
Figure 17 is the Ultra Performance Liquid Chromatography to fluorobenzene fluoroacetic acid standard solution-triple level Four bar/compounded linear ion hydrazine mass spectrogram (0.1mg/L) adopting the inventive method to obtain;
In figure, horizontal ordinate represents each plant growth regulator retention time, and ordinate represents the response intensity of each plant growth regulator.
Embodiment
Below in conjunction with embodiment, the specific embodiment of the present invention is further described.Following examples for illustration of the present invention, but are not used for limiting the scope of the invention.
1) extract
Utilize homogeneous instrument that vegetables former state is made vegetables homogenate, take 10.00g vegetables homogenate (being accurate to 0.01g) in 50mL centrifuge tube, add the acetonitrile solution of 20mL containing 1% (v/v) acetic acid, horizontal oscillations 10min, add 5.00g (being accurate to 0.01g) sodium chloride again, again vortex mixing 1min, 5000r/min off-line 3min, draw 10mL supernatant I in 15mL centrifuge tube, to be clean.
2) sample is purified
Take 100mg octadecylsilane chemically bonded silica (ODS, 60 μm) and 500mg anhydrous magnesium sulfate respectively in 10mL supernatant I, vortex mixing 2min, 5000r/min off-line 3min, Aspirate supernatant II revolves in 25mL and steams in bottle.
3) concentrated
Steaming bottle will be revolved and be placed in less than 40 DEG C water-bath concentrated by rotary evaporations to clean dry, add the acetonitrile of 1mL containing 1% (v/v) acetic acid, vortex oscillation, dissolve to revolve and steam residue in bottle, filter membrane (0.22 μm of lipophilicity Nylon 66 Membrane) measures for UHPLC-QTRAP after filtering.
4) UHPLC-QTRAP condition determination
Chromatographic column: C18,50 × 2.1mm (internal diameter), 1.7 μm, or suitable person;
Mobile phase: acetonitrile-2mmol/L ammonium acetate buffer, gradient elution program is as follows:
Positive ion mode:
Negative ion mode:
Each Compound Retention time: in table 1;
Mass spectrometry parameters: in table 1;
Column temperature: 40 DEG C;
Flow velocity: 0.3mL/min;
Sample size: 10 μ L;
Prerun time: 1.0min;
Positive ion mode total run time: 5min;
Negative ion mode total run time: 6min;
Ultra Performance Liquid Chromatography-triple level Four bar/compounded linear ion hydrazine mass spectroscopy
The content of middle measured object per sample, the matrix working solution that selected peak area is close.In matrix working solution and sample liquid, the response of each plant growth regulators all should in certain range of linearity.Ion relative abundance in sample solution, compared with the ion relative abundance in matrix matching standard solution, meets the requirement of table 2.Matrix working solution and sample liquid equal-volume intert sample introduction measure, under above-mentioned chromatographic condition, the reference retention time of each target compound is shown in middle table 1.Ultra Performance Liquid Chromatography-triple level Four bar/compounded linear ion hydrazine the mass spectrogram of 17 plant growth regulators standard solution is see Fig. 1 ~ Figure 17.
The permissible variation scope of table 2 sample solution intermediate ion relative abundance
5) result calculates
With chromatographic data processor or the content pressing plant growth regulator in formula (1) calculating sample, result of calculation must deduct blank value;
In formula:
X
i---the content of test substance in sample to be tested, unit is milligrams per kilogram;
C
i---from the solution concentration of the test substance that Ultra Performance Liquid Chromatography-triple level Four bar/compounded linear ion hydrazine mass spectrogram obtains, unit is micrograms per millilitre;
V---the final constant volume of sample liquid, unit is milliliter;
M---final sample to be tested quality representated by sample liquid, unit is gram.
The plant growth regulator to be measured adding 2.0 μ g/kg concentration levels in export vegetable carries out recovery test, and the average recovery rate that replicate determination is 6 times and relative standard deviation are in table 3.
Table 3 mark-on average recovery rate and relative standard deviation
As can be seen from above example, the embodiment of the present invention is detected various plants growth regulator in export vegetable by solvent extraction, purification, concentrate etc., and method has higher sensitivity, accuracy and precision.
Claims (3)
1. the Simultaneously test method of various plants growth regulator in export vegetable, is characterized in that, comprise the steps:
1) extract
Add vegetables homogenate and contain the acetonitrile solution of 1% acetic acid in centrifuge tube, the ratio of the acetonitrile solution of 1% acetic acid is contained in the homogenate of every 1g vegetables and 2mL, horizontal oscillations 10min, the ratio of 0.5g sodium chloride is added again in the homogenate of every 1g vegetables, add sodium chloride in centrifuge tube, the centrifugal 3min of vortex mixing 1min, 5000r/min, Aspirate supernatant I is in centrifuge tube, to be clean;
2) sample is purified
Be equipped with in the centrifuge tube of supernatant I described in octadecylsilane chemically bonded silica and anhydrous magnesium sulfate being added by weight 1:5, the centrifugal 3min of vortex mixing 2min, 5000r/min, Aspirate supernatant II steams in bottle in revolving;
3) concentrated
To revolve steaming bottle and be placed in less than 40 DEG C water-bath concentrated by rotary evaporations to clean dry, add the acetonitrile of 1mL containing 1% acetic acid, vortex oscillation, dissolving is revolved and is steamed residue in bottle, after membrane filtration, measures for UHPLC-QTRAP;
4) UHPLC-QTRAP measures, and condition determination is as follows:
Chromatographic column: C18;
Mobile phase: acetonitrile-2mmol/L ammonium acetate buffer, gradient elution;
The reference retention time of each compound and mass spectrometry parameters, in table 1, are wherein with * to represent qualitative ion and quota ion;
Column temperature: 40 DEG C;
Flow velocity: 0.3mL/min;
Sample size: 10 μ L;
Prerun time: 1.0min;
Positive ion mode total run time: 5min;
Negative ion mode total run time: 6min;
Obtain UHPLC-QTRAP figure;
The reference retention time of table 1 17 plant growth regulators and mass spectrometry parameters
5) result calculates
With chromatographic data processor or the content pressing plant growth regulator in formula (1) calculating sample, result of calculation must deduct blank value;
In formula:
X
i---the content of test substance in sample to be tested, unit is milligrams per kilogram;
C
i---from the solution concentration of the test substance that UHPLC-QTRAP figure obtains, unit is micrograms per millilitre;
V---the final constant volume of sample liquid, unit is milliliter;
M---final sample to be tested quality representated by sample liquid, unit is gram.
2. the Simultaneously test method of various plants growth regulator in export vegetable according to claim 2, is characterized in that: step 4) described in the elution program of gradient elution as follows:
Positive ion mode:
Negative ion mode:
3. the Simultaneously test method of various plants growth regulator in export vegetable according to claim 1, is characterized in that: step 3) described filter membrane selects 0.22 μm of lipophilicity Nylon 66 Membrane.
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