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Residue testing method for levamisole hydrochloride in different tissues of aquatic product

A technology of levamisole hydrochloride and a detection method, which is applied in the direction of measuring devices, instruments, scientific instruments, etc., can solve the problems of human health hazards, residues, and detection method system research that have not been reported, so as to reduce reagent waste, improve recovery rate, Detecting the effects of faster analysis

Inactive Publication Date: 2015-10-28
FISHERIES SCI RES INST OF JILIN PROVINCE
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  • Summary
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  • Description
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AI Technical Summary

Problems solved by technology

[0008] Among the existing pretreatment methods for levamisole hydrochloride residues, the detection methods of levamisole hydrochloride residues in tissues such as pigs, cattle, and chickens have been reported but few, and there are no systematic studies on the detection methods of residues in aquatic products in various tissues. See the report
With the application of levamisole hydrochloride in the aquaculture industry, if the drug is not used correctly and reasonably in the breeding process, it will cause its residue and cause harm to human health.

Method used

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  • Residue testing method for levamisole hydrochloride in different tissues of aquatic product
  • Residue testing method for levamisole hydrochloride in different tissues of aquatic product
  • Residue testing method for levamisole hydrochloride in different tissues of aquatic product

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0055] Embodiment 1. Ultra-high performance liquid chromatography conditions--a comparative experiment of mobile phases with different ratios.

[0056] (1) Chromatographic conditions other than mobile phase

[0057] Instrument: Waters ACQUITY UPLC (with UV detector);

[0058] Chromatographic column: Waters BEH C18 (2.1mm×50mm, particle size 1.7μm);

[0059] Column temperature: 35°C;

[0060] Injection volume: 5 μL.

[0061] UV detection wavelength: 214nm.

[0062] Flow rate: 0.4mL / min;

[0063] (2) Different mobile phase composition

[0064] The ratios of phosphoric acid solution at pH 7.0 to acetonitrile were 90:10, 85:15, and 80:20, respectively.

[0065] (3) Results

[0066] Chromatographic analysis results such as image 3 , as shown in the figure, when the mobile phase changes, the chromatographic peak changes accordingly, and the pH=7.0 phosphoric acid solution is selected in this experiment. The ratio of phosphoric acid solution and acetonitrile in the mobile p...

Embodiment 2

[0067] Embodiment 2. Comparison of chromatographic behavior of levamisole hydrochloride on UPLC and traditional HPLC.

[0068] (1) UPLC chromatographic conditions

[0069] Instrument: Waters ACQUITY UPLC (with UV detector);

[0070] Chromatographic column: Waters BEH C18 (2.1mm×50mm, particle size 1.7μm);

[0071] Mobile phase: 0.05mol / L phosphoric acid (adjust pH to 7 with triethylamine): acetonitrile=85:15(V / V);

[0072] Column temperature: 35°C;

[0073] Injection volume: 5 μL.

[0074] UV detection wavelength: 214nm.

[0075] Flow rate: 0.4mL / min;

[0076] (2) HPLC chromatographic conditions

[0077] Instrument: Waters 1525 (with UV detector);

[0078] Chromatographic column: Waters symmetry C18 (4.6mm×150mm, particle size 5μm);

[0079] Mobile phase: 0.05mol / L phosphoric acid (adjust pH to 7 with triethylamine): acetonitrile=75:25(V / V);

[0080] Column temperature: 35°C;

[0081] Injection volume: 20 μL.

[0082]UV detection wavelength: 214nm.

[0083] Flow ra...

Embodiment 3

[0094] Embodiment three, the comparison of levamisole hydrochloride extractant in the aquatic product plasma.

[0095] (1) Chromatographic conditions

[0096] Instrument: Waters ACQUITY UPLC (with UV detector);

[0097] Chromatographic column: Waters BEH C18 (2.1mm×50mm, particle size 1.7μm);

[0098] Mobile phase: 0.05mol / L phosphoric acid (adjust pH to 7 with triethylamine): acetonitrile=85:15(V / V);

[0099] Column temperature: 35°C;

[0100] Injection volume: 5 μL.

[0101] UV detection wavelength: 214nm.

[0102] Flow rate: 0.4mL / min;

[0103] (2) Experimental steps

[0104] Accurately draw 1 mL of the plasma sample and place it in a 15 mL centrifuge tube, add 1 mL of borate buffer (pH=9) to the centrifuge tube, then add 10 mL of ethyl acetate / acetonitrile to the centrifuge tube, vortex for 2 minutes, Centrifuge in a centrifuge at 4000r / min for 5 minutes, transfer the supernatant in the centrifuge tube to a BUCHI 48-position parallel evaporator vacuum tube; add 5 mL...

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Abstract

The invention provides a residue testing method for levamisole hydrochloride in different tissues of an aquatic product, and belongs to the technical field of levamisole hydrochloride detection methods. The method comprises the steps of 1, setting the basic value of an ultraviolet detector of an ultra-high performance liquid chromatograph (UPLC); 2, extracting the residue of levamisole hydrochloride in the plasma of an aquatic product; 3, extracting the residues of levamisole hydrochloride in the muscle, the hepatopancreas and the kidney of the aquatic product; 4, determining the content of levamisole hydrochloride in the aquatic product. According to the technical scheme of the invention, pre-treatment technologies are optimized and rationally combined, so that the extraction and purification effect is ensured to be good. Meanwhile, the condition of the UPLC is explored and confirmed, and the sensitivity, the repeatability and the accuracy of the detection method are improved. Especially, the detection and analysis speed is accelerated by several times, and the reagent waste is lowered. The environmental pollution is reduced. The method is suitable for the residue detection of great batch of samples.

Description

technical field [0001] The invention belongs to the technical field of detection methods for levamisole hydrochloride, in particular to a detection method for detecting levamisole hydrochloride in aquatic product tissues by using ultra-high performance liquid chromatography. Background technique [0002] Levamisole hydrochloride, English name: Levamisole Hydrochloride, molecular formula: C11H12N2S·ClH, molecular weight: 240.757, chemical structure as figure 1 shown. Chinese alias: (S)-6-phenyl-2,3,5,6-tetrahydro-imidazol[2,1-B]thiazole monohydrochloride; L-2,3,5,6-tetrahydro- 6-Phenylimidazol[2,1-6]thiazole hydrochloride; Anthelmintic speed; Levotetramisole; (S)-(-)-6-Phenyl-2,3,5,6-tetrahydroimidazo [2,1-b]thiazole hydrochloride; levamisole hydrochloride; L-2,3,5,6-tetrahydro-6-phenylimidazo(2,1-B)thiazole hydrochloride; hydrochloric acid Levamisole. [0003] Levamisole hydrochloride is the L-isomer of tetramisole, and its activity is about 1 to 2 times that of tetramis...

Claims

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Application Information

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IPC IPC(8): G01N30/88
Inventor 李改娟刘艳辉祖岫杰周井祥戴欣鞠松柏杜晓燕陈伟强刘慧吉殷微赵全东
Owner FISHERIES SCI RES INST OF JILIN PROVINCE
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