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Method for detecting nitrofuran veterinary drugs in shrimp flesh

A technology of nitrofuran and detection method, which can be applied to measurement devices, instruments, scientific instruments, etc., can solve the problems of cumbersome and complicated detection process, shortened derivatization time, and low detection efficiency, and achieves the advantages of shortened time, rapid response and high sensitivity. Effect

Pending Publication Date: 2021-08-31
XINJIANG UNIVERSITY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] The purpose of the present invention is to provide a method for the determination of nitrofuran drugs in shrimp meat, so as to solve the problem that the existing national standard GB / T 21311-2007 has a long pretreatment time and a cumbersome detection process in the pretreatment process of meat products Complexity and low detection efficiency, and a relatively cheap liquid chromatography-fluorescence detection method was established to detect samples, while ensuring high sensitivity, it greatly shortened the derivatization time and simplified the detection steps, and the obtained detection results were stable and reliable

Method used

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  • Method for detecting nitrofuran veterinary drugs in shrimp flesh
  • Method for detecting nitrofuran veterinary drugs in shrimp flesh
  • Method for detecting nitrofuran veterinary drugs in shrimp flesh

Examples

Experimental program
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Effect test

Embodiment 1

[0041] Weigh 2.00 g of homogeneous shrimp meat sample into a 50 mL centrifuge tube, add 10 mL of 0.2 mol / L HCl, vortex for 2 min, place the sample in a constant temperature ultrasonic reactor at 40 °C for 20 min, and then Centrifuge at 6000 r / min for 5 min, remove 5 mL of supernatant, and concentrate the supernatant at 50 °C under nitrogen protection.

[0042] Add 50 uL of 8 mmol / L 4-dianilinobenzaldehyde, 200 uL of acetonitrile and 200 uL of aqueous hydrochloric acid at pH=1.0 to the concentrated solution in sequence, vortex for 2 min, and place the mixed reaction solution at 50 °C Derivatize and mark in a constant temperature ultrasonic reactor for 20 min. After derivatization, add 50 uL, 0.5 mol / L NaOH to neutralize the acidity and alkalinity of the reaction solution, and vortex for 1 min. Centrifuge at a high speed for 10 min, pipette the supernatant to pass through the membrane, and then test it on the machine.

Embodiment 2

[0044] Weigh 1.00 g of homogeneous shrimp meat sample into a 50 mL centrifuge tube, add 5 mL of 0.2 mol / L HCl, vortex for 2 min, place the sample in a constant temperature ultrasonic reactor at 40 °C for 20 min, and then Centrifuge at 6000 r / min for 5 min, remove all the supernatant, and concentrate the supernatant at 50°C under nitrogen protection.

[0045]Add 50 uL of 8 mmol / L 4-dianilinobenzaldehyde, 200 uL of acetonitrile and 200 uL of aqueous hydrochloric acid at pH=1.0 to the concentrated solution in sequence, vortex for 2 min, and place the mixed reaction solution at 50 °C Derivatize and mark in a constant temperature ultrasonic reactor for 20 min. After derivatization, add 50 uL, 0.5 mol / L NaOH to neutralize the acidity and alkalinity of the reaction solution, and vortex for 1 min. Centrifuge at a high speed for 10 min, pipette the supernatant to pass through the membrane, and then test it on the machine.

Embodiment 3

[0047] Weigh 2.00 g of homogeneous shrimp meat sample into a 50 mL centrifuge tube, add 10 mL of 0.2 mol / L HCl, vortex for 2 min, place the sample in a constant temperature ultrasonic reactor at 60 °C for 10 min, and then Centrifuge at 6000 r / min for 5 min, remove 5 mL of supernatant, and concentrate the supernatant at 60 °C under nitrogen protection.

[0048] Add 50 uL of 8 mmol / L 4-dianilinobenzaldehyde, 200 uL of acetonitrile and 200 uL of aqueous hydrochloric acid at pH=1.0 to the concentrated solution in sequence, vortex for 2 min, and place the mixed reaction solution at 50 °C Derivatize and mark in a constant temperature ultrasonic reactor for 20 min. After derivatization, add 50 uL, 0.5 mol / L NaOH to neutralize the acidity and alkalinity of the reaction solution, and vortex for 1 min. Centrifuge at a high speed for 10 min, pipette the supernatant to pass through the membrane, and then test it on the machine.

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Abstract

The invention discloses an UPLC-FLD analysis method for rapidly detecting nitrofuran metabolite residues in shrimp flesh. The analysis method comprises the following steps: 1) adding an acid aqueous solution into a homogenized shrimp flesh sample, performing dissociating under ultrasound waves, and carrying out centrifuging to obtain a supernatant A; 2) concentrating the supernatant A under the protection of nitrogen to obtain a concentrated sample B; 3) sequentially adding a fluorescent derivatization reagent, acetonitrile and a aqueousdilute acid solution into the concentrated sample B, and carrying out auxiliary derivatization under constant-temperature ultrasound waves; and 4) carrying out low-temperature high-speed centrifugation on a derived solution, allowing the derived solution to pass through a membrane, and performing testing on a machine. According to the method, nitrofuran metabolite and a new fluorescent derivatization reagent are subjected to rapid derivatization by using a constant-temperature ultrasonic-assisted derivatization technology, and finally, a fluorescent detector is used for detection. In a pretreatment process, derivatization reaction time is greatly shortened, the use of organic reagents is greatly reduced, and operation steps are simple and efficient; and in addition, the high-fluorescence derivatization reagent can obviously improve detection sensitivity, and rapid, simple and accurate detection of nitrofuran veterinary drugs is achieved.

Description

[0001] field of invention [0002] The invention relates to a method for detecting veterinary drugs in food. Specifically, the invention relates to a method for determining nitrofuran veterinary drug residues in shrimp meat. Background technique [0003] Shrimp meat is widely loved by consumers because it is light and refreshing, and rich in protein, fat, carbohydrates, calcium, iron, phosphorus and other nutrients. my country is the largest producer of prawn farming in the world. The export of prawns has maintained a steady growth in recent years. However, in the process, the number of notifications from relevant departments due to the detection of prohibited veterinary drugs has also increased relatively, especially regarding the Nitrofuran veterinary drug residues. Nitrofuran drugs are a class of artificially synthesized broad-spectrum antibiotics. They were widely used in shrimp farming to prevent and treat gastroenteritis and other animal diseases in the early days. Howe...

Claims

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Application Information

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IPC IPC(8): G01N30/02G01N30/06G01N30/74
CPCG01N30/02G01N30/06G01N30/74
Inventor 王吉德王康康寇钰丽王猛
Owner XINJIANG UNIVERSITY
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