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Method for measuring indazole flusulfamide residue amount

A technology for determination of indazole sulfasulfame and its determination method, which is applied in the field of determination of indazole sulfasulfame residue, can solve problems such as no detection method for indazole sulfasulfame residue, and achieve avoidance of matrix interference and good repeatability , the effect of high sensitivity

Active Publication Date: 2013-11-27
青岛海润农大检测有限公司
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  • Abstract
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  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] With the registration, promotion and use of indazole sulfasulfame, countries such as Japan, the United States, the European Union and South Korea, which are the main export markets of vegetables and fruits in my country, have established residue limit standards for it, stipulating that it is present in a variety of vegetables and fruits. The maximum allowable residue is 0.01 ~ 3 mg / kg, but there is no report on the detection method of indazole sulfasulfame residue at home and abroad

Method used

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  • Method for measuring indazole flusulfamide residue amount
  • Method for measuring indazole flusulfamide residue amount
  • Method for measuring indazole flusulfamide residue amount

Examples

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Embodiment 1

[0037] Embodiment 1: the detection of the residual amount of indazole sulfamethamine in seasoning sauce

[0038] (1) Sample pretreatment

[0039] Weigh 10.0 g of well-mixed seasoning sauce into a 50 mL centrifuge tube, accurately add 20 mL of acetonitrile, homogeneously extract for 1 min, add 3 g of anhydrous magnesium sulfate and 2 g of sodium chloride, and centrifuge at 5000 r / min for 5 min . After centrifugation, take 2 mL of acetonitrile extract and transfer to a medium containing 200 mg anhydrous magnesium sulfate, 100 mg C 18 and 50 mg PSA in a centrifuge tube, vortex for 1 min, and centrifuge at 5000 r / min for 3 min. The supernatant was taken and passed through a 0.22 μm filter membrane for determination.

[0040] (2) Preparation of standard working solution

[0041] Accurately weigh 25±0.1 mg of the standard product in a 25 mL volumetric flask, dissolve it with acetonitrile, and dilute to the volume to obtain a 1000.0 μg / mL standard stock solution; pipette 1.0 mL ...

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Abstract

The invention discloses a method for measuring indazole flusulfamide residue amount. The method comprises the following steps: homogenizing and extracting residual indazole flusulfamide in a sample by using acetonitrile or 1 percent of acetic acid-acetonitrile, dispersing and purifying the extracting solution through an ethidene diamine-N-propoxysilane (PSA) and octadecyl silane bonded phase (C18) matrix, performing liquid chromatography-tandem mass spectrometry (LC-MS / MS) detection, establishing a corrected standard curve by adopting dilution standards of a blank matrix solution, and quantifying through an external standard method. According to the method, the average recovery rate is 84.2-91.4 percent, the average relative standard deviation (RSD) is 3.7-6.6 percent, the detection limit is 1.53mu g / kg, and the method has the advantages of simplicity and convenience in operation, high rapidness, high accuracy, high sensitivity and high repeatability. The technical requirements on the safety detection of corresponding products in European Union, USA, Korea, Japan, Taiwan and other countries can be met, and powerful technical support is provided for guaranteeing the food safety of people in China and the export abroad trade health development.

Description

technical field [0001] The present invention relates to a method for determining the residual amount of indazole, more specifically, qualitative and quantitative determination of residual indazole in vegetables, fruits and their products by using high performance liquid chromatography-tandem mass spectrometry (LC-MS / MS) The invention discloses a method for the content of sulfanil, which belongs to the technical field of determination of pesticide residues. Background technique [0002] In recent years, my country's agricultural product export has grown rapidly and has become an important part of my country's foreign trade. Among them, the export volume of vegetables has jumped to the first place in the world, and the production and export of fruits are also in the forefront of the world. However, with the continuous expansion of the planting area of ​​vegetables and fruits and the improvement of the multiple cropping index, the occurrence and damage of pests and diseases ar...

Claims

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Application Information

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IPC IPC(8): G01N30/88
Inventor 崔淑华郭庆龙范昆王松辛学谦王建华王境堂
Owner 青岛海润农大检测有限公司
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