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Rapid detection method of cyromazine in vegetables

A detection method, the technology of cyromazine, applied in the field of pesticide detection, can solve the problems of unsatisfactory detection effect of cyromazine residues, low detection sensitivity, long sample injection time, etc., achieve excellent standard addition recovery rate, simple operation, save The effect of the time of injection

Inactive Publication Date: 2020-03-17
日照健安检测技术服务有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The detection sensitivity of the instrument used in this method is low, it can only be quantified according to the peak time, and the injection time is long, so the detection effect of cyromazine residues is not ideal, the recovery rate is low and the detection speed is slow

Method used

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  • Rapid detection method of cyromazine in vegetables
  • Rapid detection method of cyromazine in vegetables
  • Rapid detection method of cyromazine in vegetables

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0054] Prepare 8 stoppered centrifuge tubes, numbered 1-6, of which No. 1 is the whole blank, No. 2 is the base blank, and No. 3-8 is the standard addition.

[0055] Crush the blank matrix spinach sample, mix well, accurately weigh 5g (accurate to 0.01g) into centrifuge tubes No. Add 100ng cyromazine standard solution to No. 7-8 centrifuge tubes respectively, add 200 ng cyromazine standard solution to No. about 5g anhydrous Na 2 SO 4 , 2gNaCL, centrifuge at 4000r / min for 5min, and take 1mL of the supernatant for purification.

[0056] Place a strong cation exchange column (SCX) in a solid-phase extraction device, pre-rinse with 5mL of methanol for activation, and then equilibrate with 5mL of water. When the solvent reaches the surface of the column adsorption layer, immediately transfer 1mL of the above-mentioned solution to be purified to the SCX column. Wash the SCX column successively with 2% formic acid water and 6 mL of methanol, discard the effluent and drain the smal...

Embodiment 2

[0058] Prepare 8 stoppered centrifuge tubes, numbered 1-6, of which No. 1 is the whole blank, No. 2 is the base blank, and No. 3-8 is the standard addition.

[0059] Crush the blank matrix cabbage sample, mix well, accurately weigh 5g (accurate to 0.01g) into No. 2-6 centrifuge tubes with stoppers, add 50ng cyromazine standard solution to No. Add 100ng cyromazine standard solution to No. 7-8 centrifuge tubes respectively, add 200ng cyromazine standard solution to No. 7-8 centrifuge tubes respectively, add 25mL2% acetic acid acetonitrile in 8 centrifuge tubes, add about 5g anhydrous Na 2 SO 4 , 2gNaCL, centrifuge at 4000r / min for 5min, and take 1mL of the supernatant for purification.

[0060] Place a strong cation exchange column (SCX) in a solid-phase extraction device, pre-rinse with 5mL of methanol for activation, and then equilibrate with 5mL of water. When the solvent reaches the surface of the column adsorption layer, immediately transfer 1mL of the above-mentioned sol...

Embodiment 3

[0062] Prepare 8 stoppered centrifuge tubes, numbered 1-6, of which No. 1 is the whole blank, No. 2 is the base blank, and No. 3-8 is the standard addition.

[0063] Crush the blank matrix green bean sample, mix well, accurately weigh 5g (accurate to 0.01g) in centrifuge tubes No. Add 100ng cyromazine standard solution to No. 6 centrifuge tubes respectively, add 200 ng cyromazine standard solution to No. 7-8 centrifuge tubes respectively, add 25mL2% acetic acid acetonitrile in 8 centrifuge tubes, homogenize (8000r / min) while Add about 5g anhydrous Na 2 SO 4 , 2gNaCL, centrifuge at 4000r / min for 5min, and take 1mL of the supernatant for purification.

[0064] Place a strong cation exchange column (SCX) in a solid-phase extraction device, pre-rinse with 5mL of methanol for activation, and then equilibrate with 5mL of water. When the solvent reaches the surface of the column adsorption layer, immediately transfer 1mL of the above-mentioned solution to be purified to the SCX col...

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Abstract

The invention, which belongs to the technical field of pesticide detection, discloses a rapid detection method of cyromazine in vegetables. The detection method comprises the following steps: crushinga vegetable sample and fully and uniformly mixing the sample; accurately weighing the vegetable sample and putting the vegetable sample into a centrifugal tube; adding 2% of acetic acid acetonitrile;carrying out homogenizing by using a homogenizer and adding anhydrous Na2SO4 and NaCL during the process of homogenizing; carrying out centrifuging; taking 1mL of supernatant for purification after centrifuging; and carrying out qualitative and quantitative analysis on the treated sample in a high performance liquid chromatography-mass spectrometer to obtain the content of cyromazine in the vegetables. The method has the beneficial effects that the chromatographic peak response of cyromazine in the detection method is good; the peak can appear within 2.37 minutes and the instrument response is high, so that the sample injection time is effectively saved and the detection efficiency of cyromazine is improved; the detection accuracy of cyromazine is obviously improved in the detection method; the adding standard recovery rate of a sample is between 90.01% and 104.81%; and the relative standard deviation is between 0.50% and 3.49%.

Description

technical field [0001] The invention relates to the technical field of pesticide detection, in particular to a rapid detection method for cyromazine in vegetables. Background technique [0002] Cyromazine (Cyromazine) has another name called cyromazine, and its chemical name is N-cyclopropyl-1,3,5-triazine-2,4,6-triamine, which is a kind of triazine compound, which is harmful to insects It is a new type of high-efficiency, low-toxicity, nitrogen-containing heterocyclic insecticide, which plays a role in regulating growth. It has special physiological activity for preventing and controlling Diptera insect larvae and pupae. Its morphology is distorted, resulting in the inhibition or incomplete emergence of adults, so as to achieve the purpose of controlling the excessive reproduction of dipteran pests and reducing the number of pests. [0003] At present, in my country, cyromazine residues in vegetables are very serious, and the existing detection standard of cyromazine in ve...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N30/88G01N30/06
CPCG01N30/06G01N30/88G01N2030/062G01N2030/884
Inventor 成艳彭桂芝刘祥燕张廷翠曹慧艳郭晓华郑萌萌秦瑶张永勤
Owner 日照健安检测技术服务有限公司
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