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Method for measuring residual quantity of prothioconazole and metabolite prothioconazole-desthio thereof in apples

A technology of thioconazole and prothioconazole is applied in the field of determination of prothioconazole and its metabolite thioconazole residues in apples, which can solve the problem of difficulty in effective extraction and detection, instability of prothioconazole To achieve the effect of saving sample pretreatment time and cost, meeting limited detection requirements, and fast analysis speed

Active Publication Date: 2020-12-15
合肥海关技术中心 +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] Based on the existing problems in the above-mentioned prior art, the object of the present invention is to provide a method for determining the residual amount of prothioconazole and its metabolite thioketoconazole in apples, so as to solve the problem that prothioconazole is unstable and difficult to obtain in apples. The technical problems of effective extraction and detection, to realize the rapid extraction, purification and accurate qualitative and quantitative determination of prothioconazole and its metabolite thioketoconazole residues in apples

Method used

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  • Method for measuring residual quantity of prothioconazole and metabolite prothioconazole-desthio thereof in apples
  • Method for measuring residual quantity of prothioconazole and metabolite prothioconazole-desthio thereof in apples
  • Method for measuring residual quantity of prothioconazole and metabolite prothioconazole-desthio thereof in apples

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0033] Step 1. Sample preparation

[0034] Put the apple samples (above 500g) in the refrigerator at 2°C for 2 hours, take out the samples and remove the handle, cut the whole fruit into pieces quickly in the dark and mix them well, put them into a grinder, add an appropriate amount of dry ice and crush them all to obtain samples.

[0035] Step 2. Extraction

[0036] Weigh 5g of the sample (accurate to 0.01g), put it into a 50mL stoppered brown centrifuge tube, quickly add 10mL of 15μg / mL ascorbic acid aqueous solution and vortex to mix, then add 10mL of formic acid acetonitrile solution with a volume concentration of 1%, Vortex extraction for 2 min; add 5 g of sodium chloride to the centrifuge tube, vortex for 1 min; centrifuge at 5000 r / min at 4°C for 5 min, and take the supernatant to be purified.

[0037] Step 3. Purification

[0038] Put 1.0 mL of the supernatant obtained in step 2 into a container containing 50 mg C 18 , 50 mg PSA and 150 mg anhydrous magnesium sulfat...

Embodiment 2

[0048] Step 1. Sample preparation

[0049] Put the apple samples (above 500g) in the refrigerator at 4°C for 2 hours, take out the samples and remove the handle, cut the whole fruit into pieces quickly in the dark and mix them well, put them into a grinder, add an appropriate amount of dry ice and crush them all to obtain samples.

[0050] Step 2. Extraction

[0051] Weigh 5g sample (accurate to 0.01g), put it into a 50mL stoppered brown centrifuge tube, quickly add 10mL 20μg / mL ascorbic acid aqueous solution and vortex mix, then add 10mL formic acid acetonitrile solution with a volume concentration of 1%, Vortex extraction for 2 min; add 5 g of sodium chloride to the centrifuge tube, vortex for 1 min; centrifuge at 4000 r / min at 4°C for 5 min, and take the supernatant to be purified.

[0052] Step 3. Purification

[0053] Put 1.0 mL of the supernatant obtained in step 2 into a container containing 100 mg C 18 , 50 mg PSA and 150 mg anhydrous magnesium sulfate in a 2 mL cen...

Embodiment 3

[0064] Step 1. Sample preparation

[0065] Put the apple samples (above 500g) in the refrigerator at 2°C for 2 hours, take out the samples and remove the handle, cut the whole fruit into pieces quickly in the dark and mix them well, put them into a grinder, add an appropriate amount of dry ice and crush them all to obtain samples.

[0066] Step 2. Extraction

[0067] Weigh 5g of the sample (accurate to 0.01g), put it into a 50mL stoppered brown centrifuge tube, quickly add 10mL of 15μg / mL ascorbic acid aqueous solution and vortex to mix, then add 10mL of formic acid acetonitrile solution with a volume concentration of 1%, Vortex extraction for 2 min; add 5 g of sodium chloride to the centrifuge tube, vortex for 1 min; centrifuge at 8000 r / min at 4°C for 5 min, and take the supernatant to be purified.

[0068] Step 3. Purification

[0069] Put 1.0 mL of the supernatant obtained in step 2 into a container containing 50 mg of C 18 , 50mgPSA and 200mg anhydrous magnesium sulfat...

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Abstract

The invention discloses a method for measuring residual quantity of prothioconazole and metabolite prothioconazole-desthio thereof in apples, which comprises the steps of removing the stem of a refrigerated apple sample to be measured, dicing the apple sample in a dark place, adding dry ice, and pulverizing to obtain a sample; and sequentially adding an ascorbic acid aqueous solution, an acetonitrile formate solution and sodium chloride into the sample, carrying out vortex oscillation extraction, centrifuging, purifying the obtained supernatant, diluting, and carrying out UHPLC-MS / MS analysisso as to determine the residual quantity of prothioconazole and the metabolite prothioconazole-desthio thereof in the sample. The technical problem that prothioconazole in apples is difficult to extract and detect effectively is solved, the method can be used for rapid extraction, purification and accurate qualitative and quantitative analysis of the residual quantity of prothioconazole and metabolite prothioconazole-desthio of prothioconazole in apples, and the method is sensitive and high in accuracy.

Description

technical field [0001] The invention belongs to the technical field of enrichment, purification and detection of pesticide residues in food, and in particular relates to a method for determining the residues of prothioconazole and its metabolite thioketoconazole in apples. Background technique [0002] Pesticide residue analysis is an analytical technique for trace components in complex mixtures. Less sample consumption, less reagent consumption and faster analysis are the development trend of pesticide chemical pollutant residue detection technology. How to realize multi-residue analysis and ensure the recovery rate while effectively removing impurities is the difficulty of the whole pretreatment process. [0003] In recent years, prothioconazole has been widely used in agricultural products such as grains, and its main metabolite in plant-derived foods is Prothioconazole-desthio. The Codex Alimentarius Commission (CAC) stipulates that the residue limit of prothioconazole...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N30/88G01N30/06
CPCG01N30/88G01N30/06
Inventor 宋伟韩芳许曼曼侯建波吕亚宁刘宇欣丁磊周典兵赵霞郑平
Owner 合肥海关技术中心
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