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A kind of hplc detection method of octocalid residue in food

A detection method, the technology of octoprodil, is applied in the field of HPLC detection of octoprodil residues in food, which can solve the problems of insufficient literature and achieve the effects of good repeatability, avoiding matrix interference and high practicability

Active Publication Date: 2020-09-25
梅里埃检测技术(青岛)有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

At present, there is no detection standard for octoprobin residues in food, and there are not many literatures

Method used

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  • A kind of hplc detection method of octocalid residue in food
  • A kind of hplc detection method of octocalid residue in food
  • A kind of hplc detection method of octocalid residue in food

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0045] The HPLC detection of octocalid residual amount in the concentrated apple juice of embodiment 1:

[0046] (1) Weighing of the sample: Weigh 2 g of concentrated apple juice (accurate to 0.01 g), then add 2 mL of 1mol / L sodium bicarbonate, and shake to completely wet and disperse the sample.

[0047] (2) Extraction of the sample: Add 4 mL of 1 mol / L sodium bicarbonate solution and 4 mL of acetonitrile to the sample in step (1), shake well, and extract by ultrasonic for 30 min.

[0048] (3) Derivatization reaction: Add 0.3 mL of 0.1% Fmoc-Cl derivatization solution and shake well. If the acetonitrile layer is found to be less than 4 mL, about 2 g of sodium chloride should be added to the extract. Let stand for 10 minutes, shake twice in the middle, centrifuge at 3500 rpm / min for 3 minutes, filter the organic phase through a 0.22 µm filter membrane into a sample vial for HPLC analysis.

[0049] (4) Configuration of the standard curve: Standard stock solution: Accurately w...

Embodiment 2

[0059] The HPLC detection of octocalid residual amount in the apple powder of embodiment 2:

[0060] (1) Weighing of the sample: Weigh 1 g (accurate to 0.01 g) of apple powder, then add 2 mL of 1 mol / L sodium bicarbonate, shake to completely wet the sample, and soak overnight.

[0061] (2) Sample extraction: Add 4 mL of 1 mol / L sodium bicarbonate solution and 4 mL of acetonitrile to the sample soaked overnight in step (1), shake well, and extract by ultrasonic for 30 min.

[0062] (3) Derivatization reaction: Add 0.3 mL of 0.1% Fmoc-Cl derivatization solution and shake well. If the acetonitrile layer is found to be less than 4 mL, about 2 g of sodium chloride should be added to the extract. Let stand for 10 minutes, shake twice in the middle, centrifuge at 3500 rpm / min for 3 minutes, filter the organic phase through a 0.22 µm filter membrane into a sample vial for HPLC analysis.

[0063] The configuration of the standard curve, high-performance liquid chromatography (HPLC) d...

Embodiment 3

[0067] The HPLC detection of octocalid residual amount in embodiment 3 tomato paste:

[0068] (1) Weighing of the sample: Weigh 1 g of tomato paste (accurate to 0.01 g), then add 2 mL of 1 mol / L sodium bicarbonate, and shake to completely wet and disperse the sample

[0069] (2) Sample extraction: Add 4 mL of 1 mol / L sodium bicarbonate solution and 4 mL of acetonitrile to the sample soaked overnight in step (1), shake well, and extract by ultrasonic for 30 min.

[0070](3) Derivatization reaction: Add 0.3 mL of 0.1% Fmoc-Cl derivatization solution and shake well. If the acetonitrile layer is found to be less than 4 mL, about 2 g of sodium chloride should be added to the extract. Let stand for 10 minutes, shake twice in the middle, centrifuge at 3500 rpm / min for 3 minutes, filter the organic phase through a 0.22 µm filter membrane into a sample vial for HPLC analysis.

[0071] The configuration of the standard curve, high-performance liquid chromatography (HPLC) determination...

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Abstract

The invention relates to the field of detection of pesticide residues and provides an HPLC detection method for octocalid residues in food. The sample of the present invention is extracted by sodium bicarbonate solution and acetonitrile, derivatized by Fmoc-Cl derivative solution, and measured by high performance liquid chromatography, and the chromatographic peak area of ​​the standard working solution is used for regression analysis of its corresponding concentration to obtain the standard working curve, external standard Quantitative method, the measured average recovery rate is 68%-117%, and the average relative standard deviation (RSD) is 0.7%-8.2%, with high sensitivity and good repeatability. The detection limit is 0.001 mg / kg, the quantitative detection limit of concentrated apple juice is 0.01 mg / kg, and the quantitative detection limit of apple powder, tomato paste, tomato powder and rapeseed is 0.05 mg / kg, compared with GB 2763‑2016 In the maximum residue limit of pesticides in food, the limit requirements for octocalid in tomato, apple and cottonseed are 0.5 mg / kg, 0.1 mg / kg and 0.1 mg / kg respectively, and the detection limit and quantification limit of the present invention are lower. The technical scheme of the invention has the characteristics of quickness, simplicity and high practicability, and can fully meet the requirements of pesticide residue detection.

Description

technical field [0001] The invention relates to the field of detection of pesticide residues, in particular to an HPLC detection method for octocalid residues in food. Background technique [0002] The chemical name of octoprodil is N, N-di-n-octyldiethylenetriamine, which is a broad-spectrum, low-toxic fungicide developed in my country, and has significant killing effects on various plant fungi, bacteria and viruses that cause crop diseases. extinction and inhibition. It is suitable for various diseases of tobacco, apple, rice, pepper and cotton, especially the control of virus diseases. In GB 2763-2016 Maximum Residue Limits of Pesticides in Food, the limit requirements for octocalid in tomato, apple and cottonseed are 0.5mg / kg, 0.1mg / kg and 0.1mg / kg respectively. At present, there is no detection standard for octocalidin residues in food, and there are not many literatures. [0003] Cycloprodil is a kind of alkylpolyamine fungicide, its structural formula is as follows:...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): G01N30/02G01N30/06G01N30/14G01N30/74G01N30/88
CPCG01N30/02G01N30/06G01N30/14G01N30/74G01N30/88G01N2030/027G01N2030/062G01N2030/146G01N2030/8809
Inventor 赵春华邓锁成张伟伟付萌王永春
Owner 梅里埃检测技术(青岛)有限公司
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