Method for rapidly detecting residual quantity of 4-hydroxycoumarin rodenticide by using distributed solid phase extraction

A hydroxycoumarin, dispersed technology, applied in the direction of measuring devices, material separation, analysis of materials, etc., can solve the problems of consuming a large amount of solvents and long processing steps, and achieve the effects of solvent saving, low detection limit, and small interference

Inactive Publication Date: 2013-08-21
谱尼测试集团股份有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The pretreatment steps are long and consume a lot of solvent

Method used

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  • Method for rapidly detecting residual quantity of 4-hydroxycoumarin rodenticide by using distributed solid phase extraction
  • Method for rapidly detecting residual quantity of 4-hydroxycoumarin rodenticide by using distributed solid phase extraction
  • Method for rapidly detecting residual quantity of 4-hydroxycoumarin rodenticide by using distributed solid phase extraction

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0025] Using methanol as the solvent, prepare the stock solutions of four rodenticides, mirfafeum, rodenticide, brodifafeum, and flumarumone, respectively, according to Table 1, and prepare mixed standard solutions, and perform UPLC-MS / MS based on the above experimental conditions. MS analysis detection. figure 1 It is the extracted ion chromatogram of the four detected rodenticides, the ordinate in the chromatogram represents the relative instrument corresponding value of the peak, and the abscissa is the retention time, in minutes. Depend on figure 1 It can be seen that the peak times of the four rodenticides are 3.35, 3.59, 5.04, and 4.59 minutes respectively, and they can be separated well. Make a graph with the peak area against the concentration to establish a standard curve for the four rodenticides, such as figure 2 As shown, the abscissa in the standard curve is the concentration of the target substance, and the ordinate is the response value of the liquid chromato...

Embodiment 2

[0032]Accurately weigh 10g of cucumber sample into a 50ml plastic centrifuge tube, add an appropriate amount of acetonitrile, add an appropriate amount of glacial acetic acid to acidify, add an appropriate amount of filler anhydrous sodium acetate, anhydrous magnesium sulfate, etc. to a 50ml centrifuge tube, and vortex first to mix 1min, then placed in the ultrasonic instrument, ultrasonic at room temperature for 5 minutes. Then, it was refrigerated and centrifuged at 4000 g for 5 min at 4 °C. Take the supernatant and transfer it into a 2ml small centrifuge tube, add an appropriate amount of purification filler anhydrous magnesium sulfate and amino adsorbent, refrigerate and centrifuge at a speed above 6000g for 5 minutes, take the supernatant, pass it through the membrane, and run it on the machine for liquid chromatography-tandem mass spectrometry detection . Two parallel samples were made for this sample, and the target substance was not detected in the sample. The stabil...

Embodiment 3

[0036] The standard solution in Example 1 was added to the vegetables in Example 2, and the experiment was carried out according to the pretreatment method and instrumental analysis and detection method of the above-mentioned samples. Three concentration spike experiments were done on this sample, and the samples of each spiked concentration were measured in parallel three times, and the average value of the three measurements was taken. According to the amount of reagent added and the actual measurement results, the recovery rate of the sample was calculated. The experimental results are shown in Table 4. It can be seen from Table 4 that the recovery rate of the samples is between 96-129%.

[0037] Table 4 The recovery of standard addition of this sample

[0038]

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PUM

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Abstract

The invention relates to a method for rapidly detecting a residual quantity of a 4-hydroxycoumarin rodenticide by using a distributed solid phase extraction. The method comprises pre-treating the detected samples by using the distributed solid phase extraction method, and detecting by using an ultra-high performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS), wherein the sample pre-treatment comprises fully dispersing samples with chloralkane, alcohol and ester solvents, adding proper fillers such as anhydrous sodium acetate, anhydrous magnesium sulfate, etc., performing vortex ultrasonic, centrifuging, taking a supernatant, adding a purifying agent for complete purification, and detecting the centrifuged and purified liquid with UPLC-MS/MS; separating conditions of the UPLC-MS/MS comprises using a C18 reversed phase chromatography, and having a column temperature being 30-60 DEG C, an injection volume being 2-10 [mu]l, and a flow velocity of a mobile phase being 0.15-0.60 ml/min; and detection conditions of the tandem mass spectrometry MS/MS comprises using an electrospray ion source, a negative ionization mode to ionize and a multiple reaction monitoring mode. The method provided by the invention has characteristics of quick extraction and purification, high method selectivity, strong chromatogram specificity and little interference.

Description

【Technical field】: [0001] The present invention designs a detection method for the residual amount of 4-hydroxycoumarin rodenticides, especially relates to the purification of dispersed solid phase extraction, and detects 4-hydroxycoumarin by means of ultra-high performance liquid chromatography-quadrupole tandem mass spectrometer method for rodenticide residues. 【Background technique】: [0002] 4-Hydroxycoumarin rodenticide is a kind of slow-acting rodenticide commonly used at home and abroad, and is considered to be a relatively ideal anticoagulant drug. Rodenticides are mainly divided into two types according to their chemical structures: one is based on 4-hydroxycoumarin, and the other is based on indandione. Although the two types of compounds have different chemical structures, they have the same mechanism of action. All of them can competitively inhibit vitamin K in rats and hinder the synthesis of prothrombin, resulting in fatal internal hemorrhage and death. [0...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N30/89
Inventor 宋薇
Owner 谱尼测试集团股份有限公司
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