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Method for detecting residual quantity of spinosad A, spinosad D, clothianidin and thiamethoxam in zucchini

A spinosyn and detection method technology, which is applied to the detection of residues of thiamethoxam, clothianidin, spinosad A and spinosad D in zucchini, can solve the problem of time-consuming, cumbersome, and untested samples. Problems such as the complexity of the pre-processing process to achieve the effect of improving sensitivity and resolution and shortening the pre-processing time

Inactive Publication Date: 2020-11-20
安徽华辰检测技术研究院有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, the main problems in these methods are that the pretreatment process of the samples to be tested is complex, cumbersome, and time-consuming, which brings great pressure to the detection work.
In addition, there is no detection method for the simultaneous detection of clothianidin, thiamethoxam, spinosyn A and D. Quantitative changes, research is needed to find a convenient and reliable method

Method used

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  • Method for detecting residual quantity of spinosad A, spinosad D, clothianidin and thiamethoxam in zucchini
  • Method for detecting residual quantity of spinosad A, spinosad D, clothianidin and thiamethoxam in zucchini
  • Method for detecting residual quantity of spinosad A, spinosad D, clothianidin and thiamethoxam in zucchini

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Experimental program
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Effect test

Embodiment 1

[0052] A method for detecting residues of spinosad A, spinosad D, clothianidin, and thiamethoxam in zucchini, which is detected by liquid chromatography tandem mass spectrometer LCMS-8050 from Shimadzu Corporation of Japan, wherein the high performance liquid phase The chromatographic conditions are: the chromatographic column is a Shim-pack XR-ODSⅡ chromatographic column (2.0mmi.d×75mm), the mobile phase A is 0.1% formic acid aqueous solution with a volume fraction, the mobile phase B is acetonitrile, and the flow rate is 0.3mL / min. The column temperature was 38°C, the injection volume was 1 μL, and gradient elution was performed.

[0053] The gradient elution program is: within 0-1.00min, the proportion of mobile phase A is 80%, and the proportion of mobile phase B is 20%; within 1.00-3.00min, the proportion of mobile phase A gradually changes from 80% to 10% ; Within 3.00-4.00min, the proportion of mobile phase A is maintained at 10%; within 4.00-4.01min, the proportion of ...

Embodiment 2

[0088] Embodiment 2 recovery test

[0089] By adding a sample of known concentration, the residual amount of spinosyn A, spinosyn D, clothianidin, and thiamethoxam in the sample was detected according to the method and detection conditions of Example 1, and the recovery rate was calculated.

[0090] experiment procedure:

[0091] Take the zucchini blank matrix, weigh 6 parts, each weighs 2.000g, numbered A, B, C, D, E, F, then take spinosad A, spinosad D, clothianidin, clothianidin The standard stock solution of zine (same as Example 1) was diluted to different concentrations respectively, added to A, B, C, D, E, F zucchini blank matrix, mixed uniformly, so that in A, B samples, spinosad A, The added concentrations of spinosyn D, clothianidin, and thiamethoxam were 0.05mg / kg, 0.05mg / kg, 0.06mg / kg, and 0.05mg / kg in sequence; D, clothianidin, thiamethoxam added concentration is 0.2mg / kg, 0.2mg / kg, 0.5mg / kg, 0.5mg / kg; The added concentration of amine and thiamethoxam was 1mg / k...

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Abstract

The invention discloses a method for detecting the residual quantity of spinosad A, spinosad D, clothianidin and thiamethoxam in zucchini, which adopts a high performance liquid chromatography-mass spectrometry method for detection and uses a convenient pretreatment method. An addition and recovery test is carried out on the zucchini matrix, the recovery rate of spinosad A is 84-95%, and the RSD is 1.7-3.1%; the recovery rate of spinosad D is 93%-99%, and the RSD is 0.7%-3.7%; the recovery rate of the thiamethoxam is 87-101%, and the RSD is 1.4-3.6%; and the recovery rate of clothianidin is 87%-118%, and the RSD is 0.8%-1.5%. According to the method, the residual quantity of spinosad A, spinosad D, clothianidin and thiamethoxam in the zucchini can be simply, conveniently, quickly and accurately detected.

Description

technical field [0001] The invention relates to the technical field of pesticide residue detection, in particular to a method for detecting residues of spinosyn A, spinosyn D, clothianidin and thiamethoxam in zucchini. Background technique [0002] Spinosyn, also known as spinosad, is a macrolide pollution-free and efficient biopesticide extracted from the fermentation broth of Saccharopolyspora spinosa. The main active ingredient of spinosad has two structures, namely, spinosad Baccidin A and spinosyn D, as the receptors of nicotinic acid acetylcholine receptors, can continuously activate the target acetylcholine nicotinic receptors, and have rapid contact and stomach poisoning effects on pests. [0003] Both thiamethoxam and clothianidin belong to the neonicotinoids, which are a new class of efficient, safe, and highly selective insecticides. Their effects are similar to those of nicotinic acid acetylcholine receptors, and they have contact, stomach toxicity, and systemic ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N30/02G01N30/06G01N30/86
CPCG01N30/02G01N30/06G01N30/8675
Inventor 王小明刘松乔琳朱玉杰
Owner 安徽华辰检测技术研究院有限公司
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