CN102269696A - Detection method of dithiocarbamate pesticide residue - Google Patents
Detection method of dithiocarbamate pesticide residue Download PDFInfo
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- CN102269696A CN102269696A CN201010197943XA CN201010197943A CN102269696A CN 102269696 A CN102269696 A CN 102269696A CN 201010197943X A CN201010197943X A CN 201010197943XA CN 201010197943 A CN201010197943 A CN 201010197943A CN 102269696 A CN102269696 A CN 102269696A
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- dithiocarbamate pesticide
- dithiocarbamate
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Abstract
The invention relates to a detection method of dithiocarbamate pesticide residue, which solves false positive problems generated in present detection methods of the dithiocarbamate pesticide residue with colourimetry. The detection method of the dithiocarbamate pesticide residue comprises the following steps: 1, homogenizing a sample, heating cruciferous crops and the like to slight boil to allow interferents containing sulfur to evaporate, adding graphite powder and sodium chloride to crops with dark colors, and homogenizing to adsorb pigments; 2, adding the processed sample to a distillation apparatus, adding a reaction reagent, and heating and simultaneously accessing nitrogen to allow carbon disulfide decomposed by the dithiocarbamate pesticide residue to be carried into a receiver tube; and 3, preparing a work curve, and quantificationally detecting sample liquids by an ultraviolet-visible spectrophotometer with 5cm cuvettes at a wavelength of 435nm. According to the present invention, the detection method which is simple and easy to operate is adopted to eliminate interferences in colourimetry detection, so the method has the advantages of accuracy and reliability, and convenient popularization.
Description
Technical field:
The present invention relates to a kind of detection method of dithiocarbamate pesticide residue
Background technology:
As extensively being used as the dithiocarbamate agricultural chemicals that germifuge uses, its metabolin is found carcinogenic and effect teratogenesis, now formulated the highest value of limiting the quantity of control by more and more countries and use, mainly contain headspace sampling-vapor-phase chromatography (importing and exporting the detection of dithiocarbamate pesticide residue in the fruit as SN/T0157-1992) and ultraviolet spectrometry colourimetry (as the research of quick detection method for dithiocarbamate pesticide residue in the agricultural product such as tealeaves such as king family of Food Science institute of University Of Agriculture and Forestry In Fujian is clever, wangdan is red) at its detection method.The required instrument of vapor-phase chromatography is expensive, ultraviolet spectrometry colorimetric ratio juris all is that the dithiocarbamate agricultural chemicals is resolved into carbon disulphide, react qualitative and quantitative analysis by carbon disulphide and developer, but we find that in the actual detected process the method has false positive and occurs, analyzing reason is because part agricultural product (for example crop in cruciferae) itself contain sulfide, this sulfide meeting and chromogenic reagent, the interference characterisation quantitative test; The darker food of some color can take color in the receiving tube to when pre-treatment in addition, disturbs normally and analyzes.
Summary of the invention:
The present invention is improved on the basis of ultraviolet spectrometry colourimetry, and detection method accurately and reliably a kind of and with low cost is provided;
The detection method of dithiocarbamate pesticide residue of the present invention is as follows: (1) pulverizes equal quality sample; (2), get quantitative sample and add water heating little 15-25 of boiling minute for crop in cruciferae such as Chinese cabbage, radish; For the darker sample of colors such as purple perilla, get that quantitative sample adds an amount of dag and sodium chloride stirs, pickled 40-60 minute; Other samples are only pulverized homogeneous, all forward among the flask c; (3) assemble distilling apparatus by figure, in first absorption tube, add 5-8% NaOH 15mL; Add 0.4-0.6g/L Schweinfurt green-ethanolic solution 1mL and 10g/L diethanolamine-ethanolic solution 15mL equally respectively at second, third, in the 4th absorption tube; (4) this flask is put into 70-75 ℃ of water-bath, adds 4g SnCl2.2H2O, 200mL pure water therein, with the logical nitrogen of 0.5-0.8mL/min; (5) after the hydrochloric acid 200mL (6) of the 1.5M that has just boiled by the slow adding of separating funnel simultaneously distills 30-60 minute in 70-75 ℃ of water-bath, with second, third, the solution of the 4th absorption tube changes with ethanol and hold in the 25mL color comparison tube; (7) at 435nm wavelength place, the drawing standard curve carries out sample detection to the ultraviolet-visible spectrophotometer with the 5cm cuvette.
The improvements of the present invention and other ultraviolet spectrometry colourimetrys: because of part agricultural product (for example crop in cruciferae) itself contain sulfide, the interference measurement in the receiving tube of can vaporizing during distillation, the decomposition temperature that the present invention finds the dithiocarbamate agricultural chemicals is more than 190C ° and not volatile, and by evidence dithiocarbamate agricultural chemicals under little 15-25 minute condition of boiling be difficult for decomposing, volatilization, and the sulfide of interference measurement can effectively volatilize; For the darker crop of color, can take color to during distillation and disturb colorimetric estimation in the receiving tube, even carry out the sample blank test, also can influence method sensitivity more deeply because of the background color; The present invention adopts dag and sodium chloride particle and the sample homogeneous that adds certain particle size range by a large amount of tests, and pickles at normal temperatures 40-60 minute, makes the abundant adsorpting pigment of dag, and color can not be brought in the absorption tube in still-process subsequently.
The comparison of the present invention and conventional ultraviolet spectrometry
Annotate: the sample blank that conventional method detects purple cabbage promptly has obvious color
Mark-on recovery test data of the present invention
Description of drawings:
Accompanying drawing is an installation drawing of the present invention.
Embodiment:
Embodiment 1: the Chinese cabbage sample
(1) pulverizes equal quality sample, get the 50.0g sample and added the water heated and boiled 15 minutes, forward among the flask c;
(2) assemble distilling apparatus by figure, in first absorption tube, add 6.5% NaOH 15mL; Add 0.5g/L Schweinfurt green-ethanolic solution 1mL and 10g/L diethanolamine-ethanolic solution 15mL equally respectively at second, third, in the 4th absorption tube;
(3) this flask is put into 70-75 ℃ of water-bath, adds 4g SnCl2.2H2O, 200mL pure water therein, with the logical nitrogen of 0.6mL/min, and the hydrochloric acid 200mL of the 1.5M that has just boiled by the slow adding of separating funnel simultaneously;
(4) distillation after 30 minutes in 70-75 ℃ of water-bath is with second, third, the solution of the 4th absorption tube changes with ethanol and hold in the 25mL color comparison tube;
(5) at 435nm wavelength place, the drawing standard curve carries out sample detection to the ultraviolet-visible spectrophotometer with the 5cm cuvette.
Embodiment 2: the Chinese cabbage sample
(1) pulverizes equal quality sample, get the 100.0g sample and added the water heated and boiled 20 minutes, forward among the flask c;
(2) other steps are identical to (5) with the step (2) of embodiment 1 with parameter.
Embodiment 3: the Chinese cabbage sample
(1) pulverizes equal quality sample, get the 100.0g sample and added the water heated and boiled 25 minutes, forward among the flask e;
(2) other steps are identical to (5) with the step (2) of embodiment 1 with parameter.
Embodiment 4: the purple perilla sample
(1) pulverizes equal quality sample, get that the 50.0g sample adds the 5g dag and 40g sodium chloride stirs, pickled 60 minutes; Forward among the flask c
(2) other steps are identical to (5) with the step (2) of embodiment 1 with parameter.
Embodiment 5: the purple perilla sample
(1) pulverizes equal quality sample, get that the 50.0g sample adds the 10g dag and 50g sodium chloride stirs, pickled 45 minutes; Forward among the flask c
(2) other steps are identical to (5) with the step (2) of embodiment 1 with parameter.
Embodiment 6: the purple perilla sample
(1) pulverizes equal quality sample, get that the 100.0g sample adds the 30g dag and 120g sodium chloride stirs, pickled 40 minutes; Forward among the flask c
(2) other steps are identical to (5) with the step (2) of embodiment 1 with parameter.
Claims (1)
1. the detection method of a dithiocarbamate pesticide residue is characterized in that: (1) is got the 50-100g sample and is added water heating little 15-25 of boiling minute for crop in cruciferae such as Chinese cabbage, radish; For the darker sample of colors such as purple perilla, get the dag of 50-100g sample adding sample size 10-30% quality and the sodium chloride particle of sample size 80-120% quality and stir, pickled 40-60 minute; Other samples are only pulverized homogeneous; (2) distill extraction; (3) prepare working curve simultaneously and carry out colorimetric analysis.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201010197943XA CN102269696A (en) | 2010-06-01 | 2010-06-01 | Detection method of dithiocarbamate pesticide residue |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201010197943XA CN102269696A (en) | 2010-06-01 | 2010-06-01 | Detection method of dithiocarbamate pesticide residue |
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| CN102269696A true CN102269696A (en) | 2011-12-07 |
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| CN201010197943XA Pending CN102269696A (en) | 2010-06-01 | 2010-06-01 | Detection method of dithiocarbamate pesticide residue |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104142324A (en) * | 2014-07-29 | 2014-11-12 | 华南理工大学 | Method for measuring content of ethyl urethane through visible spectrophotometry |
| CN105424146A (en) * | 2015-12-11 | 2016-03-23 | 青岛市华测检测技术有限公司 | Dynamic quality metering equipment |
| CN111220602A (en) * | 2018-11-27 | 2020-06-02 | 上海尚湾信息技术有限公司 | Quick detection device of carbamate pesticide residue |
-
2010
- 2010-06-01 CN CN201010197943XA patent/CN102269696A/en active Pending
Non-Patent Citations (1)
| Title |
|---|
| 沈金灿等: "《液相色谱-串联质谱法同时测定红茶和绿茶中7种硫代氨基甲酸酯类除草剂》", 《分析化学研究简报》 * |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104142324A (en) * | 2014-07-29 | 2014-11-12 | 华南理工大学 | Method for measuring content of ethyl urethane through visible spectrophotometry |
| CN105424146A (en) * | 2015-12-11 | 2016-03-23 | 青岛市华测检测技术有限公司 | Dynamic quality metering equipment |
| CN111220602A (en) * | 2018-11-27 | 2020-06-02 | 上海尚湾信息技术有限公司 | Quick detection device of carbamate pesticide residue |
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Application publication date: 20111207 |