Method for simultaneously detecting nitrofurans raw drug residue in aquatic product

A technology for nitrofuran and aquatic products, applied in measurement devices, instruments, scientific instruments, etc., can solve the problems of increased time and cost, strict detection requirements, quantitative limits, etc., to reduce pretreatment costs, easy operation, quantitative The effect of limit increase

Inactive Publication Date: 2012-12-19
EAST CHINA SEA FISHERIES RES INST CHINESE ACAD OF FISHERY SCI
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  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Due to the wide variety of aquatic products and the complex matrix, the research on the detection method of nitrofuran technical residues in aquatic products is still relatively scarce. The existing liquid chromatography detection method for nitrofuran technical residues in aquatic products needs to use Purification by solid phase extraction, in actual operation, increases the time and cost required for pretreatment. At the same time, the quantification limit of this method is relatively high. , 10μg / kg, unable to meet the increasingly stringent testing requirements

Method used

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  • Method for simultaneously detecting nitrofurans raw drug residue in aquatic product
  • Method for simultaneously detecting nitrofurans raw drug residue in aquatic product
  • Method for simultaneously detecting nitrofurans raw drug residue in aquatic product

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0025] 1. 0.05mol / L NaH 2 PO 4 (pH=3.0) solution configuration method: weigh 7.8g NaH 2 PO 4 2H 2 Add 1000mL of ultrapure water to O, adjust the pH to 3.0 with phosphoric acid, and dilute to 1L.

[0026] 2. Preparation of four mixed standard solutions: Accurately weigh 10 mg each of furaltadone, nitrofurazone, nitrofurantoin, and furazolidone, dilute to 100 mL with methanol, prepare four mixed standard stock solutions of 100 μg / mL, and store at -20 °C. Take 1mL mixed standard stock solution, dilute to 100mL with methanol, and prepare 1μg / mL mixed standard intermediate solution. Pipette mixed standard intermediate solution, use mobile phase (volume ratio: acetonitrile: 0.05M NaH 2 PO 4 =25:75, pH3.0) to prepare standard working solutions with concentrations of 0.010, 0.015, 0.020, 0.025, 0.05, 0.1, and 0.25 μg / mL.

Embodiment 2

[0028] Sample preparation: Grass carp and large yellow croaker were descaled and skinned to take muscle along the back, pulverized by a tissue grinder, stored at -20°C, and thawed at room temperature before measurement.

[0029] Sample pretreatment:

[0030] 1 Extraction: Accurately weigh (5.00±0.05) g of the sample into a 50 mL centrifuge tube, add 8 mL of ethyl acetate, vortex for 1 min, sonicate for 5 min, vortex again for 1 min, centrifuge at 4000 r / min for 5 min, transfer the upper layer to brown In the chicken heart bottle, add 8 mL of ethyl acetate to repeat the extraction, and combine the extracts.

[0031] 2. Concentration: Concentrate the extract to dryness under reduced pressure at 30° C. on a rotary evaporator.

[0032] 3. Purification: add 2mL of n-hexane, vortex for 30s, then add 1mL of mobile phase (volume ratio: acetonitrile:0.05MNaH 2 PO 4 =25:75, pH3.0), mixed for 1min, transferred to a 10mL centrifuge tube, centrifuged at 4000r / min for 5min, took the lowe...

Embodiment 3

[0037] Chromatographic results: the standard chromatograms of four nitrofuran original drugs are shown in the attached figure 1 . The peak elution times of furaltadone, nitrofurazone, nitrofurantoin and furazolidone were 3.922, 5.294, 6.678 and 8.785 min, respectively.

[0038] Methodology Validation:

[0039] Under the experimental conditions determined by this method, use the mobile phase to prepare a standard working solution with a concentration of 0.010, 0.015, 0.020, 0.025, 0.05, 0.1, and 0.25 μg / mL, and analyze it on the machine. Take the concentration of each drug as the abscissa, The peak area is the ordinate to draw the standard curve. The experimental results show that: in the range of 0.01-0.25 μg / mL, the concentration of the nitrofuran original drug and the peak area have a good linear relationship, and the correlation coefficients are all above 0.998. The four nitrofurans Drug regression equation and correlation coefficient R 2 See Table 2.

[0040] Table 2 ...

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Abstract

The invention relates to a method for simultaneously detecting a nitrofurans raw drug residue in an aquatic product, comprising the following steps of: (1) preparing four types of mixed standard solutions; (2) preparing a sample; (3) extracting; (4) concentrating; (5) purifying; and (6) detecting. The method disclosed by the invention has the characteristics of high flexibility, simplicity and convenience in operation, low detection cost, accuracy and reliability; and the quantitative limit is 5 micrograms/kilogram and the recycling rate is more than 70%, so that the method is suitable for rapidly detecting imports and exports of the aquatic product.

Description

technical field [0001] The invention belongs to the field of quality and safety detection of aquatic products, in particular to a method for simultaneously detecting residues of nitrofuran original drugs in aquatic products. Background technique [0002] Nitrofuran drugs are synthetic antibiotics with 5-nitrofuran structure, mainly including furaltadone (Furaltadone, FTD), nitrofurazone (NFZ), nitrofurantoin (Nitrofurantoin, NFT) and furazolidone (Furazolidone, FZD). Four drugs. Because of their good antibacterial and bactericidal effects, these antibiotics have been widely used in the prevention and treatment of aquatic animal diseases. Related studies have proved that nitrofuran drugs have teratogenic, carcinogenic and mutagenic side effects. At present, countries such as the European Union, the United States, China, and Japan have banned the use of nitrofuran drugs in animal breeding. However, due to their remarkable therapeutic effect and no relevant alternative drugs,...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N30/06G01N30/02
Inventor 黄宣运于慧娟蔡友琼李冰黄冬梅史永富沈晓盛
Owner EAST CHINA SEA FISHERIES RES INST CHINESE ACAD OF FISHERY SCI
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