CN104597024A - Raman spectrometry used for rapidly detecting paraquat in fruit and vegetable on site - Google Patents
Raman spectrometry used for rapidly detecting paraquat in fruit and vegetable on site Download PDFInfo
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- CN104597024A CN104597024A CN201410717466.3A CN201410717466A CN104597024A CN 104597024 A CN104597024 A CN 104597024A CN 201410717466 A CN201410717466 A CN 201410717466A CN 104597024 A CN104597024 A CN 104597024A
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Abstract
Raman spectrometry used for rapidly detecting paraquat in fruit and vegetable on site is characterized by comprising diluting a sample (Chinese cabbage, cucumber, tomato, asparagus lettuce, pear, apple, grape, orange, etc) by using first water or deionized water according to the mass ratio of 1:1, centrifuging at room temperature at a speed of 10000-15000 rpm for 5-15 min, adsorbing the centrifuged homogenized supernatant and adding into a detection pool added with 2 mL of a detection reagent in advance, performing eddying or shaking for 0.3-1 min for homogenization, and performing rapid quantitative and qualitative determination on trace paraquat residue in fruit and vegetable by employing a Raman spectrometry external standard method according to the linear corresponding relation between the Raman spectrum scattering signal intensity of paraquat at the characteristic wave number position of 1665 cm<-1> and the paraquat content. The method is simple in sample pre-treatment, low in reagent cost and easy for popularization.
Description
Technical field
The present invention relates to a kind of detection method, particularly relate to the Raman spectroscopy of paraquat field quick detection in fruits and vegetables.
Background technology
Paraquat is that quick-acting contact killing type goes out natural disposition quaternary ammonium salts herbicide, has action of contace poison and certain systemic action, can be absorbed by plant green tissues rapidly, make it withered, to the not effect of non-green tissue.Be combined and purifying with soil rapidly in soil, to plant root and perennial subterranean stem and perennial root invalid.Various annual grassy weeds can be prevented and kill off; Strong lethal effect is had to perennial weeds, but its subterranean stem and root energy eruption shoot; On lignified brown stem and trunk without impact.Be applicable to prevent and kill off the weeds in orchard, mulberry field, plantation and forest belt, also can be used for the weeds of preventing and kill off bare place, ridge, roadside, for the wide row crop in corn, sugarcane, soybean and nursery, directed spraying management of weeds can be taked.
Zoopery belongs to medium malicious class, but higher to people's toxicity, and adult estimates that lethal quantity 20% aqueous solution is about 5 ~ 15ml or about 40mg/kg.It is that acute human is poisoned to death one of the highest herbicide of rate, and reported death nearly hundreds of example abroad, how to have been wrongly taken by per os lethal, 49 examples wherein wrongly taking 20% more than aqua 30ml are all dead.Intoxicating mechanism is not yet illustrated at present, most scholar thinks that paraquat is an electron accepter, can be absorbed in cell by lung I type and II type cell active transport, act on the redox reaction of cell, on the basis of intracellular activation to be oxygen radical be toxic action, the excessive super oxide anion free radical (O=) formed and hydrogen peroxide (H
2o
2) etc. can cause lung, liver and other many histoorgan Cell membrane lipids peroxidating, thus cause the infringement of multisystem histoorgan.
The detection method of current paraquat comprises chromatography, ultraviolet spectrophotometry, ELISA method etc., and sample pre-treatments comprises extraction (backflow, filtration, extraction etc.), crosses the step such as column purification, wash-out, and operating process is numerous and diverse, takes time and effort.
Surface enhanced raman spectroscopy, can make the sensitivity of spectral analysis improve 10
2~ 10
7doubly.This quick, direct spectral technique, only need the sample of minute quantity, have very large application potential, its sensitivity almost reaches the level of a molecule or atom.And Surface enhanced raman spectroscopy sample-pretreating method is simple, detect rapidly, inspection cost is low, and instrument is simply portable, can be applicable to rapid field examination, detects a large amount of sample at short notice.
But use the research of Surface enhanced raman spectroscopy detection residues of pesticides less at present, there are no being applied to the report detecting fruits and vegetables paraquat.The present invention utilizes Surface enhanced raman spectroscopy technology, and set up quick, effective, simple paraquat detection method, Site Detection tool quick for residues of pesticides is of great significance.
Summary of the invention
The object of this invention is to provide a kind of method for quick to paraquat in fruits and vegetables, realize low cost, easy and simple to handle, Site Detection can be carried out, be easy to penetration and promotion, thus reach the residual Timeliness coverage of paraquat and monitoring management, overcome the problem of the residual detection very complicated of current agriculture.
Another object of the present invention is to provide a kind of detection kit used in this detection method.
A kind of Raman spectroscopy for paraquat field quick detection in fruits and vegetables, accurately take veterinary antibiotics sample edible part (Chinese cabbage, cucumber, tomato, asparagus lettuce, pears, apple, grape, orange etc.) pulverize, dilution, mixing, centrifugal, get supernatant, add in detection cell together with detection reagent, vortex or shake even, put detection cell in Portable Raman spectrometer sensing chamber, at 300 ~ 3000cm
-1scope in carry out Raman spectroscopy scans and detect and obtain Raman spectrogram, adopt Raman spectrum external standard method, according to characteristic waves 1665cm
-1place the Raman spectrum scattered signal intensity of paraquat and the linear corresponding relation of paraquat content, carry out fast quantification that in fruits and vegetables, micro-paraquat remains and qualitative detection.
For adapting to the demand, the invention provides simple fruits and vegetables pre-treating method, providing and detecting agent prescription and preparation method thereof, paraquat scene qualitative and quantitative analysis method is fast provided.Its step is as follows:
1. sample pre-treatment
Described fruits and vegetables sample, as Chinese cabbage, cucumber, tomato, asparagus lettuce, pears, apple, grape, orange, be to take at 1: 1 by the mass ratio of fruits and vegetables sample and water, preferably take fruits and vegetables sample 1g and water 1mL, mix, be placed in hydro-extractor, at room temperature centrifugal 5-15 minute under 10000 ~ 15000rpm, to be measured.Raman spectroscopy of the present invention, described water is redistilled water or deionized water.
2. detect
Be added in the detection cell having added a certain amount of reagent A and B in advance by centrifugal rear clear liquid, vortex or shake evenly, put detection cell in portable Raman spectrometer sensing chamber at 300 ~ 3000cm
-1scope in carry out Raman spectroscopy scans and obtain Raman spectrogram, as at 1665cm in Raman spectrogram
-1(wave number error < 15cm
-1) there is characteristic peak at place, then in judgement sample containing paraquat, otherwise then judge that sample is not containing paraquat.
3 reagent A are silver colloid aqueous solution, prepare according to known method; Reagent B be A can be made to condense containing C1
-1alkaline solution.
The consumption of described reagent is as follows:
(1) reagent A is detected: silver colloid aqueous solution 100 ~ 300 μ L;
(2) detect reagent B:0.5M ~ 5M ionizable go out Cl
-1alkaline solution 100 ~ 300 μ L;
(3) the application of sample amount of described fruits and vegetables sample centrifuged supernatant is 400 ~ 1200 μ L.
4. the LASER Light Source emission wavelength of Raman spectrometer of the present invention is 785nm, its wave number error < 15cm
-1, be hand-held, portable or desk-top instrument.At present, China Inst. of Quarantine Inspection Sciences, the units such as (Beijing) Science and Technology Ltd., Bi Da Imtech grind in Zhong Jian state can provide the Portable Raman spectrometer meeting test request.
When utilizing of the present invention, data acquisition and the interpretation of result step in later stage are as follows:
(1) detect with Portable Raman spectrometer, laser energy Selecting parameter 300mw, integral parameter selects 3 times, and these two parameters regulate best Raman peaks intensity, continuous sweep Raman spectrum 3 times, finally obtains the averaged spectrum of 3 scanning optical spectrums.The sweep limit of each spectrum is 300-3000cm
-1, completing a spectral scan time is 1min.
(3) Raman spectrogram of contrast feminine gender and positive fruits and vegetables sample (Chinese cabbage, cucumber, tomato, asparagus lettuce, pears, apple, grape, orange), as 1665cm
-1(wave number error < 15cm
-1) obvious Raman spectrum characteristic peak has appearred in place, and signal to noise ratio (S/N ratio)>=3, then be tentatively judged as containing the residual positive of paraquat, as characteristic waves 1665cm
-1(wave number error < 15cm
-1) place do not find obvious Raman spectrum characteristic peak, then tentatively judge sample be paraquat content lower than Monitoring lower-cut negative sample.Therefore, 1665cm
-1(wave number error < 15cm
-1) characteristic peak at place is the important evidence detecting paraquat, can carry out just size test by this characteristic peak to paraquat in fruits and vegetables sample.
(4) quantitative test: according to characteristic waves 1665cm
-1(wave number error < 15cm
-1) the linear relationship drawing standard curve of Raman scattering signal intensity corresponding to place's Paraquat and its concentration, quantified by external standard method analysis can be carried out to paraquat in fruits and vegetables with this typical curve.
Raman spectroscopy of the present invention, sample pre-treatments simple (dilution, centrifugal then can test), linear relationship is good, analysis result is intuitively visual, as used portable Raman detector then field quick detection can be realized, whether scene quantitative and qualitative detection fast can be carried out containing paraquat is residual in fruits and vegetables.
Accompanying drawing explanation
Fig. 1 is the Surface enhanced raman spectroscopy figure (0.1mg/kg) of paraquat standard items aqueous solution;
Surface enhanced raman spectroscopy figure (the A. Chinese cabbage positive of representative vegetables (Chinese cabbage) positive of Fig. 2 and negative sample; B. Chinese cabbage negative sample);
Fig. 3. representative vegetables (Chinese cabbage) add the canonical plotting of paraquat
Surface enhanced raman spectroscopy figure (the A. orange positive of representative fruit (orange) positive of Fig. 4 and negative sample; B. orange negative sample);
The representative fruit (orange) of Fig. 5 adds the canonical plotting of paraquat
Embodiment
Embodiment 1:
For a Raman spectroscopy for paraquat field quick detection in fruits and vegetables, comprise following concrete step:
1, pre-treatment: get fruits and vegetables sample (Chinese cabbage, cucumber, tomato, asparagus lettuce, apple, pears, grape, orange) and take 1g, pulverize, with water with 1: 1 dilution, mixing, centrifugal, under 15000rpm, centrifugal 10min, to be measured.
2, preparation detects reagent
(1) reagent A is detected: silver colloid aqueous solution;
(2) NaCl, NaOH aqueous solution of reagent B:1M is detected;
3, select LASER Light Source emission wavelength to be that the Portable Raman spectrometer of 785nm detects, the steps include:
(1) sample: get 100uL and detect reagent A in the detection cell of 2mL, add 100 μ L and detect reagent B, in careful aspiration step 1, centrifugal homogeneous liquid 400 μ L is in detection cell; Vortex or shake even;
(2) instrument parameter is arranged: laser energy Selecting parameter 300mw, and integral time, Selecting parameter 1 second, regulated best Raman peaks intensity by these two parameters;
(3) scan: with Raman spectrometer at 300 ~ 3000cm
-1scope in, with 13cm
-1resolution scan test sample; Read in 2 minutes or record or preserve Raman spectrum test result.Continuous sweep spectrum 3 times, finally obtains the averaged spectrum of 3 scanning optical spectrums.
5, interpretation of result
(1) just size test, by Raman spectrogram as characteristic waves 1665cm
-1(wave number error < 15cm
-1) place with or without obvious peak, then tentatively judge this sample containing paraquat remain.
(2) according to characteristic waves in Raman spectrogram 1665 (wave number error < 15cm
-1) the linear relationship drawing standard curve of raman spectral signal intensity corresponding to place and its concentration, the quantitative measurement of paraquat in fruits and vegetables is carried out according to typical curve.
Use detection reagent and the detection method of the embodiment of the present invention, adopt Portable Raman spectrometer, in multiple fruits and vegetables matrix, add paraquat, measurement result is as table 1.
Paraquat measurement result in table 1. fruits and vegetables
| Sample | Paraquat detection limit (μ g/kg) | The range of linearity (μ g/kg) | The recovery |
| Chinese cabbage | 5 | 5-100 | 82.0％(8μg/kg) |
| Cucumber | 20 | 20-80 | 106.7％(25μg/kg) |
| Tomato | 5 | 5-90 | 103.8％(8μg/kg) |
| Asparagus lettuce | 8 | 8-100 | 105.2％(15μg/kg) |
| Grape | 30 | 30-90 | 96.9％(40μg/kg) |
| Apple | 3 | 3-100 | 77.7％(8μg/kg) |
| Pears | 2 | 2-30 | 84.4％(2μg/kg) |
| Orange | 5 | 5-100 | 108.4％(8μg/kg) |
Above-described embodiment is only be described the preferred embodiment of the present invention; not scope of the present invention is limited; under not departing from the present invention and designing the prerequisite of spirit; the various distortion that the common engineering technical personnel in this area make technical scheme of the present invention and improvement, all should fall in protection domain that claims of the present invention determine.
Claims (4)
1. one kind remains the Raman spectroscopy detected fast for paraquat in fruits and vegetables, it is characterized in that: dilute sample (Chinese cabbage, cucumber, tomato, asparagus lettuce, pears, apple, grape, orange etc.) with first water or deionized water by 1: 1 mass ratio, centrifugal 5-15 minute under room temperature, 10000 ~ 15000rpm, draw centrifugal after homogeneous supernatant in the detection cell of 2mL having added detection reagent in advance, vortex or shake 0.3 ~ 1 minute homogeneous, adopt Raman spectrum external standard method, according to characteristic waves 1665cm
-1place the Raman spectrum scattered signal intensity of paraquat and the linear corresponding relation of paraquat content, carry out fast quantification that in fruits and vegetables, micro-paraquat remains and qualitative detection.
2. Raman spectroscopy according to claim 1, is characterized in that: described homogeneous supernatant sampling amount is 400 ~ 1200 μ L; Described detection reagent comprises the reagent of following consumption:
(1) reagent A is detected: silver colloid aqueous solution 100 ~ 300 μ L;
(2) detect reagent B:0.5M ~ 5M ionizable go out Cl
-1alkaline solution 100 ~ 300 μ L.
3. Raman spectroscopy according to claim 1, its operation steps is:
(1) sample: get 100-300 μ L and detect reagent A in detection cell, add 100 μ L and detect reagent B, homogeneous test solution 400,800 μ L or 1200uL after careful absorption is centrifugal is in detection cell;
(2) instrument parameter is arranged: adjust laser energy parameter and integral time parameter obtain the Raman peaks intensity of Raman spectrometer the best, adjust continuous sweep spectrum number of times, obtain best average scanning optical spectrum;
(3) scan: with Raman spectrometer at 300 ~ 3000cm
-1scope interscan test sample;
(4) interpretation of result:
1) qualitative analysis: the Raman spectrogram gathering sample to be tested, as 1665cm
-1there is obvious paraquat Raman spectrum characteristic peak in place, and signal to noise ratio (S/N ratio)>=3, then be tentatively judged as containing the residual positive of paraquat, as characteristic waves 1665cm
-1place does not find obvious paraquat Raman spectrum characteristic peak, then tentatively judge that sample is the negative sample of paraquat content lower than Monitoring lower-cut.
2) quantitative test: according to characteristic waves 1665cm
-1the linear relationship drawing standard curve of the Raman scattering signal intensity that place's Paraquat is corresponding and its concentration, can carry out quantified by external standard method analysis to paraquat in fruits and vegetables with this typical curve.
4. Raman spectroscopy according to claim 1, is characterized in that: the Raman spectrum detector used can be hand-held, portable or desk-top instrument, should possess the LASER Light Source that emission wavelength is 785nm, its wave number error < 15cm
-1, the units such as (Beijing) Science and Technology Ltd., Bi Da Imtech grind in current China Inst. of Quarantine Inspection Sciences, Zhong Jian state can provide the Portable Raman spectrometer meeting test request.
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Cited By (8)
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| CN104931483A (en) * | 2015-06-30 | 2015-09-23 | 北京工商大学 | Raman spectrum detection method for pesticide residues in fruits and vegetables |
| CN105675582A (en) * | 2016-03-22 | 2016-06-15 | 浙江大学 | Method using Raman spectrum to detect beta-carotene content in fruit |
| CN106153596A (en) * | 2015-04-13 | 2016-11-23 | 中国人民解放军军事医学科学院毒物药物研究所 | A kind of quick detection N,N'-dimethyl-.gamma..gamma.'-dipyridylium and/or the method for diquat dibromide and test kit |
| CN106770174A (en) * | 2017-01-14 | 2017-05-31 | 南京简智仪器设备有限公司 | A kind of method of utilization Raman spectrum quick detection paraquat |
| CN106814060A (en) * | 2017-01-19 | 2017-06-09 | 上海海洋大学 | A kind of method of paraquat in quick detection beverage |
| CN107238593A (en) * | 2016-03-28 | 2017-10-10 | 中检国研(北京)科技有限公司 | For diquat dibromide Raman enhanced spectrum method and its agent prescription in fruits and vegetables |
| CN108593568A (en) * | 2018-05-02 | 2018-09-28 | 上海锆仪电子科技有限公司 | Automate qualitative and quantitative material detection method, device and its system |
| CN110763533A (en) * | 2019-10-15 | 2020-02-07 | 南京简智仪器设备有限公司 | Pretreatment method suitable for detecting pesticide residues in tobacco by Raman spectrum |
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| CN106153596A (en) * | 2015-04-13 | 2016-11-23 | 中国人民解放军军事医学科学院毒物药物研究所 | A kind of quick detection N,N'-dimethyl-.gamma..gamma.'-dipyridylium and/or the method for diquat dibromide and test kit |
| CN106153596B (en) * | 2015-04-13 | 2020-01-14 | 中国人民解放军军事医学科学院毒物药物研究所 | Method for rapidly detecting paraquat and/or diquat |
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| CN105675582A (en) * | 2016-03-22 | 2016-06-15 | 浙江大学 | Method using Raman spectrum to detect beta-carotene content in fruit |
| CN107238593A (en) * | 2016-03-28 | 2017-10-10 | 中检国研(北京)科技有限公司 | For diquat dibromide Raman enhanced spectrum method and its agent prescription in fruits and vegetables |
| CN106770174A (en) * | 2017-01-14 | 2017-05-31 | 南京简智仪器设备有限公司 | A kind of method of utilization Raman spectrum quick detection paraquat |
| CN106814060A (en) * | 2017-01-19 | 2017-06-09 | 上海海洋大学 | A kind of method of paraquat in quick detection beverage |
| CN108593568A (en) * | 2018-05-02 | 2018-09-28 | 上海锆仪电子科技有限公司 | Automate qualitative and quantitative material detection method, device and its system |
| CN110763533A (en) * | 2019-10-15 | 2020-02-07 | 南京简智仪器设备有限公司 | Pretreatment method suitable for detecting pesticide residues in tobacco by Raman spectrum |
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