CN104007164A - Use of ion mobility spectrometer for detecting gibberellins residues in crops and method for detecting gibberellins residues in crops - Google Patents
Use of ion mobility spectrometer for detecting gibberellins residues in crops and method for detecting gibberellins residues in crops Download PDFInfo
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Abstract
The invention provides the use of an ion mobility spectrometer for detecting gibberellins residues in crops and a method for detecting the gibberellins residues in the crops. The uses of the ion mobility spectrometer are expanded, the thought of detecting gibberellins by using the ion mobility spectrometer is disclosed for the first time, and an implementation method for detecting the gibberellins by using the ion mobility spectrometer is provided. The gibberellins are quickly and conveniently detected, the operating method is simple, the detection sensitivity is high, and the detection result accuracy is high. The gibberellins can be detected in a laboratory as well as a supermarket and a farmers market, and law enforcement officials can implement field screening and detection conveniently.
Description
Technical field
The present invention relates to ionic migration spectrometer and agriculture residue detection technical field, relate in particular to a kind of ionic migration spectrometer for detection of the residual purposes of gibberellin in crops and method.
Background technology
Gibberellin (Gibberellins, Gas) is the plant hormone that a class belongs to diterpenoids compound, is extensively present in higher plant, fungus and bacterium, participates in each stage of regulating growth of plants.At present, from higher plant and microorganism, isolate more than 100 kind of gibberellin, generally existed with two kinds of forms of mating type to dissociate, be named as respectively GA1, GA2 ... GAn etc., are referred to as gibberellin.Wherein, gibberellic acid GA3 (Gibberellic acid) activity is the strongest, distributed more widely, is studied at most the therefore representative of Chang Zuowei gibberellin.Gibberellin GA3, has another name called 920, and formal name used at school is 2,4a, and 7-trihydroxy one 1-methyl one 8 one methylene-red are mould-3-alkene-1,10 carboxylic acids-Isosorbide-5-Nitrae-lactone, is for No. CAS 77-06-5.
The main Physiological Function of gibberellin is: promote plant cell division, cauline leaf extends, and accelerates growth and development of plants, makes crops ripen in advance, increases output, improves quality; Break vegetable seeds dormancy, promote seed, stem tuber, piece root to germinate; Improve fruit-setting rate, increase output; Extend storage period, increase fruit storage ability; Change Proportion of male and female flowers, improve seed production, produce stenospermocarpy river.Because gibberellin has above biological function, gibberellin uses very extensive on agriculture, woods, gardening, and still, abuse and excessively use meeting bring stern challenge and threat to agricultural product security.In Japan's regulation fruit, vegetables, gibberellin maximum residue limit(MRL) is 0.2 mg/kg, relates to 110 of food, and also not relevant limit standard of China.
At present the gibberellin analytical approach of bibliographical information mainly contains physical-chemical process and spectroscopy analysis method, immunoassay technology, high performance liquid chromatography, thin layer chromatography.
1. physical-chemical process and spectroscopy analysis method
Luo Guoan utilizes fluorescence spectrophotometry GA content, and gibberellin concentration has good linear relationship (r=0.999 9) within the scope of 20-164ug/mL, and average recovery rate is 100.8 scholars 1.19%.Referring to: Luo Guoan, Gu Juefen, Wang Yiming. the content [J] of fluorescence spectrophotometry gibberellin. China Medicine University's journal, 1990,21 (3): 187-188.
Holbrook is hydrolyzed under strong acidic condition based on gibberellic acid and generates the character of gibberellenic acid with uv absorption and set up gibberellin ultraviolet determination method.Referring to: HOLBROOK A A, EDGE W J W, BAILEY F.spectrophotometric method for determination of gibberellic acid[J] .Advances in Chemistry, 1961,28:159-167.
Use fluorescence spectrophotometry and determined by ultraviolet spectrophotometry gibberellin, its shortcoming is: although sensitivity is also higher, but their accuracy is all subject to the interference of impurity and reduces, and detection limit is lower, be not suitable for the mensuration of gibberellin in the comparatively complicated sample of composition.
2. immunoassay technology method
Zheng Qiuling connects mutually and prepares rabbit anti-serum with PROTEIN B SA with 7 carboxyls of reagent D CC activation GA3, and the indirect ELISA of foundation detects in conjunction with state GA3,, detection limit is 12.3ng/mL, better in 12.3～1 000 ng/mL scope internal linear.Referring to: Zheng Qiuling. in conjunction with the indirect ELISA research [J] of state GA3. Hebei Agricultural Sciences, 2010,14 (3): 154-156
The shortcoming of immunoassay technology method is: the preparation of antibody is comparatively complicated, high to requirement for experiment condition, and is prone to false-positive result.
3. chromatography
Zhou Yanming sets up the high-efficiency liquid chromatography method for detecting of Determination of Gibberellic Acid Residues in strawberry, sample adopts 80% methyl alcohol extraction, purify through liquid-liquid extraction, detect with UV-detector, it is 82.8% one 100.6% that gibberellin adds the recovery, the coefficient of variation is 3.2% one 4.6%, and minimum detectability is 0.017 mg/kg.Referring to: Zhou Yanming, Tang Yuan, Niu Sen. high performance liquid chromatography detects the research [J] of Determination of Gibberellic Acid Residues in strawberry. food industry science and technology, 2009, (30) 1:311.312,321.
Xu Qingqin etc. adopt wide bore capillary column, and without derivatization treatment, direct injected adopts the GA content in GC-FID working sample bean sprouts, and minimum detectability can reach 0.25mg/kg.Referring to: Xu Qingqin, Fan Zhefeng, Du Liming. the gibberellin ［ J ］ in heavy caliber capillary gas chromatography Fast Measurement plant tissue. Journal of Analytical Science, 2000,16 (6): 524.
Beam pendant etc. has been set up LC-MS/MS method and has been detected the gibberellin in fruit, the detection limit 0.01 μ g/L (S/N=3) of method, and the actual samples such as strawberry, apple, orange have been carried out to gibberellin residue detection, obtain good result.Referring to: beam is worn, Zhang Taozhi, Huang Honglin. and Solid-Phase Extraction/Liquid Chromatography-Tandem Mass Spectrometry method is measured the gibberellin GA3 residual ［ J ］ in fruit. analytical test journal, 2006,25 (11): 118-119.
Above-mentioned chromatographic shortcoming is: pre-treatment is loaded down with trivial details, and chemical reagent and the equipment of use are more; Chromatogram ultraviolet and chromatogram mass spectrometer are expensive, and maintenance cost is high; Liquid phase process requires high to experimental instrument and equipment, complicated operation is high to experimenter's professional knowledge requirement, wastes time and energy.
4. thin layer chromatography
Thin-layer chromatography (TLC) method is to be applied in early days a kind of method that gibberellin detects, and can separate target substance, preliminary quantitative and semi-quantitative analysis, also can detect gibberellin with fluorescent spectrometry coupling.
Thin-layer chromatography-fluorescent spectrometry that Tang Hongfang research silica G is absorption carrier, for measuring Determination of Gibberellic Acid Residues in Citrus, has good repeatability and the recovery.Referring to: Tang Hongfang, Mao Lizhen. Determination of Gibberellic Acid Residues [J] in thin-layer chromatography one fluorescence spectrum method for measuring oranges and tangerines. agricultural chemicals, 1996,35 (6): 32-33.
The shortcoming of thin layer chromatography is: complex operation, not only need to use a large amount of organic solvents, and preliminary quantitative and semi-quantitative.
Summary of the invention
For this reason, technical matters to be solved by this invention is: a kind of residual method of gibberellin in fast detecting crops is provided, detects with the rapid and convenient that realizes gibberellin, method of operating is simple, and detection sensitivity is high, and testing result accuracy rate is large.
The invention provides a kind of residual method of gibberellin in fast detecting crops, the method comprises:
Prepare the gibberellin standard solution of preset concentration gradient, and put it in ionic migration spectrometer, obtain ion mobility spectrometry spectrogram and the gibberellin typical curve of this standard solution;
Prepare crops sample solution to be measured, and put it in ionic migration spectrometer, obtain the ion mobility spectrometry spectrogram of this sample solution;
By the ion mobility spectrometry spectrogram comparison of the ion mobility spectrometry spectrogram of sample solution and standard solution, calculate the gibberellin actual content in crops sample solution to be measured according to the typical curve of gibberellin.
Wherein, the described gibberellin standard solution of preparing, comprising:
Take the gibberellin standard articles for use of preset value, with organic solvent dissolution and be diluted to preset concentration, and lucifuge stores;
When use, the gibberellin dilution of described storage is diluted to again to the gibberellin standard solution of preset concentration gradient.
Described ionic migration spectrometer is on-radiation ion gun, operating voltage is 220V/50HZ, source of the gas is independent source of the gas, for dry air, migration electric field intensity is 200 V/cm to 500V/cm, migration tube temperature is 40 DEG C to 200 DEG C, and sample introduction temperature is 170 DEG C to 250 DEG C, and sample size is 1 uL to 10uL.
Described acquisition gibberellin typical curve, comprising:
Qualitative with the relative ion mobility of gibberellin, with characteristic peak intensity or the area quantitative of gibberellin standard solution, draw the typical curve of gibberellin standard solution concentration gradient and gibberellin characteristic peak intensity or area.
Wherein, by the ion mobility spectrometry spectrogram comparison of the ion mobility spectrometry spectrogram of sample solution and standard solution, calculate the gibberellin actual content in crops sample solution to be measured according to the typical curve of gibberellin, comprising:
Qualitative with the relative ion mobility of gibberellin, with crops sample solution characteristic peak intensity to be measured or area quantitative, calculate the gibberellin actual content in crops sample solution to be measured according to the typical curve of gibberellin.
The linear equation of described typical curve is: Y=1330.4X+972.00, and R2=0.9920, wherein, and the degree of fitting of the curve that R2 represents, Y is gibberellin characteristic peak intensity, X is gibberellin concentration.
Described preparation crops sample solution to be measured, comprising:
Take crops sample to be measured, and put into centrifuge tube mesoscale eddies after adding organic solvent, put into again afterwards oscillator and vibrate;
Solution after vibration is crossed to 0.45 μ m miillpore filter, obtain described crops sample solution to be measured.
Described organic solvent is acetonitrile.
Described crops are date.
The present invention also provides a kind of ionic migration spectrometer for detection of the residual purposes of gibberellin in crops, and this purposes is: use ionic migration spectrometer and right to use to require method described in 1 to 9 any one to detect the residual of gibberellin in crops.
Ionic migration spectrometer of the present invention is for detection of the residual purposes of gibberellin in crops and method, expand the use of ionic migration spectrometer, propose for the first time to use ionic migration spectrometer to detect the idea of gibberellin, and provide the implementation method that uses ionic migration spectrometer to detect gibberellin, the rapid and convenient that has realized gibberellin detects, method of operating is simple, and detection sensitivity is high, and testing result accuracy rate is large.The detection of gibberellin both can be carried out in laboratory, also can in supermarket, the market of farm produce, carry out, be convenient to law enfrocement official's field screening and detect.
Brief description of the drawings
Fig. 1 is the residual method flow schematic diagram of gibberellin in fast detecting crops described in the embodiment of the present invention;
Fig. 2 is the typical curve of the cumulative peak intensity of gibberellin characteristic peak and concentration;
Fig. 3 is the standard feature peak of gibberellin acetonitrile solution described in the embodiment of the present invention.
Embodiment
Below, describe the present invention by reference to the accompanying drawings.
As shown in Figure 1, the present embodiment provides a kind of residual method of gibberellin in fast detecting crops, and the method comprises:
Prepare the gibberellin standard solution of finite concentration gradient, and put it in ionic migration spectrometer, obtain ion mobility spectrometry spectrogram and the gibberellin typical curve thereof of this standard solution;
Prepare crops sample solution to be measured, and put it in ionic migration spectrometer, obtain the ion mobility spectrometry spectrogram of this sample solution;
The ion mobility spectrometry standard spectrogram of the ion mobility spectrometry spectrogram of sample solution and standard solution is compared, calculate the gibberellin actual content in sample solution according to the ion mobility spectrometry typical curve of standard solution.
The present embodiment is illustrated as an example of the detection method of gibberellin in date example.
First step, need to prepare gibberellin standard solution, and this preparation method comprises:
Accurately take the gibberellin standard articles for use of preset value, with organic solvent, in the present embodiment, use acetonitrile to dissolve and be diluted to preset concentration, be stored in the vial of airtight brown lucifuge.In use, can be according to actual concentrations needs, then be diluted to the gibberellin acetonitrile standard solution of finite concentration gradient.For ensureing the precision of ion mobility spectrometry typical curve of standard solution, the precision that takes of the described gibberellin standard articles for use that accurately take preset value is generally 0.01mg.
Second step, obtains gibberellin typical curve.This preparation method comprises: draw above-mentioned gibberellin acetonitrile standard solution 4 μ L with 10 μ L micropipettors, inject or put into ionic migration spectrometer, qualitative with the relative ion mobility of gibberellin (K0), with characteristic peak intensity or the area quantitative of standard solution, the typical curve of drawing the cumulative peak intensity of concentration gradient and gibberellin characteristic peak or area, obtains gibberellin typical curve as shown in Figure 2.The linear equation of described typical curve is: Y=1330.4X+972.00, and R2=0.9920, wherein, and the degree of fitting of the curve that R2 represents, Y is gibberellin characteristic peak intensity, and the unit of characteristic peak intensity is volt, and X is gibberellin concentration.Cumulative peak is the summation of characteristic peak intensity or area.
Here, describedly qualitatively just refer to whether tested thing has gibberellin, quantitatively just refer to tested species GA content number.
Wherein, draw the dosage of gibberellin acetonitrile standard solution and determine according to the sample introduction range of capacity of ionic migration spectrometer, generally at 1-10uL.
The ionic migration spectrometer of above-mentioned use is on-radiation ion gun, operating voltage is 220V/50HZ, source of the gas is independent source of the gas, for dry air, migration electric field intensity is 200 V/cm to 500V/cm, migration tube temperature is 40 DEG C to 200 DEG C, and sample introduction temperature is 170 DEG C to 250 DEG C, and sample size is 1 uL to 10uL.
Described ionic migration spectrometer can use the ionic migration spectrometer of realizing by common ion mobility, also can use the ionic migration spectrometer of realizing by relative ion mobility.
Wherein, the ionic migration spectrometer that uses relative ion mobility to realize, by the applicant's patent No. ZL201110175660.X, denomination of invention is to utilize the method for relative ion mobility spectrometry recognition material open.And, be ZL201110212235.3 by the applicant's the patent No., denomination of invention is that ion migration ratio spectrometer is open.
Third step, prepares crops sample solution to be measured, and puts it in ionic migration spectrometer, obtains the ion mobility spectrometry spectrogram of this sample solution;
The present embodiment is taking crops date as example, weigh date 5.0g, add organic solvent, for example HPLC level acetonitrile 10mL, and the potpourri of date and acetonitrile is put into and in centrifuge tube, carried out vortex, general vortex is after 5 minutes, more described potpourri is put into oscillator vibrates, generally vibrate again 5 minutes, obtain date extract.The present embodiment centrifuge tube used is 50mL teflon centrifuge tube.
Date extract is crossed to 0.45 μ m miillpore filter, collect filtrate, as the sample solution of crops date to be measured.
Get the sample solution of 4uL crops date to be measured, put in described ionic migration spectrometer and test, the general test time is 2 minutes, ionic migration spectrometer is qualitative with the relative ion mobility (K0) of gibberellin in the sample solution of crops date to be measured, with characteristic peak intensity or area quantitative.
The 4th step, by the sample solution pyrrole urea characteristic peak superposed strength or the area that obtain in third step, in substitution gibberellin typical curve, calculates the gibberellin actual content in sample solution.Transverse axis in Fig. 3 is 1/K0, and K0 is relative ion mobility, and the longitudinal axis is gibberellin intensity.
Be specially: the ion mobility spectrometry spectrogram of the ion mobility spectrometry spectrogram of date sample solution and gibberellin standard solution is compared, qualitative with the relative ion mobility of gibberellin (K0), with actual measurement solution gibberellin characteristic peak intensity or area quantitative, calculate the actual content of gibberellin in date sample solution according to gibberellin typical curve.
In Fig. 3, there are two characteristic peaks in gibberellin collection of illustrative plates, gibberellin-1 and gibberellin-2, and in actual experiment, gibberellin-2 characteristic peak is unstable, is generally as the criterion and calculates the actual content of mycin with gibberellin-1 characteristic peak.
By foregoing description, can see, use the residual method of gibberellin in ionic migration spectrometer test crops, can realize the fast detecting of gibberellin, method of operating is simple, and detection sensitivity is high, and testing result accuracy rate is large.Overcome the pretreatment process described in background technology, with an organic solvent, for example acetonitrile, can directly carry out the extraction of test fluid to crops, and whole testing process is consuming time is less than 10 minutes.And ionic migration spectrometer instrument performance is stable, automaticity is high.Tester can detection on duty through simple training, both can carry out in laboratory, also can be in supermarket, the market of farm produce and law enforcement related personnel carry out examination test.
The embodiment of the present invention also provides a kind of ionic migration spectrometer for detection of the residual purposes of gibberellin in crops, this purposes is: use ionic migration spectrometer and use the residual method of gibberellin in the use ionic migration spectrometer test crops described in above-described embodiment, detect the residual of gibberellin in crops.
The purposes that the present embodiment provides, open up a new use of ionic migration spectrometer, in the detection of gibberellin, propose for the first time to use ionic migration spectrometer to detect the idea of gibberellin, and provided the concrete methods of realizing that uses ionic migration spectrometer detection gibberellin.
In sum, described in the present embodiment, ionic migration spectrometer is for detection of the residual purposes of gibberellin in crops and method, expand the use of ionic migration spectrometer, propose for the first time to use ionic migration spectrometer to detect the idea of gibberellin, and provided the implementation method that uses ionic migration spectrometer to detect gibberellin, and the rapid and convenient that has realized gibberellin detects, and method of operating is simple, detection sensitivity is high, and testing result accuracy rate is large.The detection of gibberellin both can be carried out in laboratory, also can in supermarket, the market of farm produce, carry out, be convenient to law enfrocement official's field screening and detect.
The foregoing is only preferred embodiment of the present invention, in order to limit the present invention, within the spirit and principles in the present invention not all, any amendment of doing, be equal to replacement, improvement etc., within all should being included in protection scope of the present invention.
Claims (10)
1. the residual method of gibberellin in fast detecting crops, is characterized in that, comprising:
Prepare the gibberellin standard solution of preset concentration gradient, and put it in ionic migration spectrometer, obtain ion mobility spectrometry spectrogram and the gibberellin typical curve of this standard solution;
Prepare crops sample solution to be measured, and put it in ionic migration spectrometer, obtain the ion mobility spectrometry spectrogram of this sample solution;
By the ion mobility spectrometry spectrogram comparison of the ion mobility spectrometry spectrogram of sample solution and standard solution, calculate the gibberellin actual content in crops sample solution to be measured according to the typical curve of gibberellin.
2. method according to claim 1, is characterized in that, the described gibberellin standard solution of preparing, comprising:
Take the gibberellin standard articles for use of preset value, with organic solvent dissolution and be diluted to preset concentration, and lucifuge stores;
When use, the gibberellin dilution of described storage is diluted to again to the gibberellin standard solution of preset concentration gradient.
3. method according to claim 1, it is characterized in that, described ionic migration spectrometer is on-radiation ion gun, operating voltage is 220V/50HZ, and source of the gas is independent source of the gas, is dry air, migration electric field intensity is 200 V/cm to 500V/cm, migration tube temperature is 40 DEG C to 200 DEG C, and sample introduction temperature is 170 DEG C to 250 DEG C, and sample size is 1 uL to 10uL.
4. method according to claim 1, is characterized in that, described acquisition gibberellin typical curve, comprising:
Qualitative with the relative ion mobility of gibberellin, with characteristic peak intensity or the area quantitative of gibberellin standard solution, draw the typical curve of gibberellin standard solution concentration gradient and gibberellin characteristic peak intensity or area.
5. method according to claim 1, it is characterized in that, by the ion mobility spectrometry spectrogram comparison of the ion mobility spectrometry spectrogram of sample solution and standard solution, calculate the gibberellin actual content in crops sample solution to be measured according to the typical curve of gibberellin, comprising:
Qualitative with the relative ion mobility of gibberellin, with crops sample solution characteristic peak intensity to be measured or area quantitative, calculate the gibberellin actual content in crops sample solution to be measured according to the typical curve of gibberellin.
6. method according to claim 5, is characterized in that, the linear equation of described typical curve is: Y=1330.4X+972.00, and R2=0.9920, wherein, and the degree of fitting of the curve that R2 represents, Y is gibberellin characteristic peak intensity, X is gibberellin concentration.
7. method according to claim 1, is characterized in that, described preparation crops sample solution to be measured, comprising:
Take crops sample to be measured, and put into centrifuge tube mesoscale eddies after adding organic solvent, put into again afterwards oscillator and vibrate;
Solution after vibration is crossed to 0.45 μ m miillpore filter, obtain described crops sample solution to be measured.
8. according to the method described in claim 1 to 7 any one, it is characterized in that, described organic solvent is acetonitrile.
9. according to the method described in claim 1 to 8 any one, it is characterized in that, described crops are date.
10. ionic migration spectrometer, for detection of the residual purposes of gibberellin in crops, is characterized in that, uses ionic migration spectrometer and uses method described in the claims 1 to 9 any one to detect the residual of gibberellin in crops.
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| CN105675708A (en) * | 2016-01-27 | 2016-06-15 | 武汉矽感科技有限公司 | Method for detecting 17beta-estradiol in water by ionic mobility spectrometer |
| CN109781893A (en) * | 2019-02-22 | 2019-05-21 | 中华全国供销合作总社济南果品研究院 | A kind of method of Rapid identification red date slices quality and processing method |
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| CN109781893A (en) * | 2019-02-22 | 2019-05-21 | 中华全国供销合作总社济南果品研究院 | A kind of method of Rapid identification red date slices quality and processing method |
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