Fast extraction and LC-MS-MS detection method of benzimidazole and thiazole type residual medicine in aquatic product

A technology of LC-MS-MS and residual drugs, which is applied in the field of quality and safety of aquatic products, can solve problems such as environmental pollution, a large amount of waste liquid and waste gas, and achieve the ideal of less extraction and purification steps, saving manpower and material resources, and perfect peak output Effect

Inactive Publication Date: 2017-06-20
YANGTZE RIVER FISHERIES RES INST CHINESE ACAD OF FISHERY SCI
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  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

At present, the extraction methods used in these detection methods still remain in liquid-liquid extraction and solid-phase extraction, which require a lot of manpower and a long time for sample processing, and a large amount of organic reagents are used in the processing methods, resulting in a large amount of waste. liquid and waste gas, causing pollution to the environment

Method used

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  • Fast extraction and LC-MS-MS detection method of benzimidazole and thiazole type residual medicine in aquatic product
  • Fast extraction and LC-MS-MS detection method of benzimidazole and thiazole type residual medicine in aquatic product
  • Fast extraction and LC-MS-MS detection method of benzimidazole and thiazole type residual medicine in aquatic product

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0030] Embodiment 1: the effect comparison of different extraction solvents

[0031] (1) Extraction: Weigh 2 g of the bream muscle blank sample into a 50 mL centrifuge tube, add the mixed standard solution of the compound to be tested in the blank sample, and make each compound to be tested (LEV, MBZ-NH 2 , MBZ-OH, MBZ, ABZ-SO, ABZ-SO 2 、ABZ-NH 2 -SO 2 and ABZ) to a final concentration of 2, 3 and 4 μg / kg, respectively, adding internal standard deuterated albendazole (ABZ-D 3 ) and deuterated mebendazole (MBZ-D 3 ), so that the final concentration reaches 5 μg / kg and 10 μg / kg respectively, add 0.84g magnesium sulfate (add 0.44g, 0.84g and 1.04g magnesium sulfate respectively in the extraction sample, and find that when adding 0.84g magnesium sulfate, the extract can be completely Blow dry to achieve the best effect) and 0.21g sodium chloride, add 10mL extraction solvent, vortex for 1min, centrifuge at 5000rpm for 5min, take 5.5mL extract, and set aside;

[0032] In this e...

Embodiment 2

[0058] Embodiment 2: the effect comparison of different cleaning agents

[0059] According to the method described in Example 1, with acetonitrile as the extraction solvent, respectively choose C18 powder (octadecylsilane), PSA powder (ethylenediamine-N-propylsilane), AL-N powder (neutral alumina ), NH 2 powder ((aminopropyl) silica gel matrix), C18+AL-N mixed powder (50mg each) as purifiers, compare the effect of different purifiers on LEV, MBZ-NH 2 , MBZ-OH, MBZ, ABZ-SO, ABZ-SO 2 、ABZ-NH 2 -SO 2 and ABZ assay effects.

[0060] Such as figure 2 , 3 , 4, choose C18 powder, PSA powder, NH 2 When the powder was used to purify the extract, a large interference peak appeared when the levamisole quantitative ion 91.3 was detected; the AL-N powder was selected as the purifying agent, and the impurity peak was eliminated; Figure 5 As shown, the final purification of each compound through C18 and AL-N mixed powder (each 50mg) can reach a higher recovery rate, and there are f...

Embodiment 3

[0061] Embodiment 3: the comparison of the pH value of aqueous phase to the peak-out effect of levamisole

[0062] According to the method described in Example 1, with acetonitrile as the extraction solvent, select C18+AL-N mixed powder (each 50mg) as the purifying agent, add ammonium acetate 10mmol / L in the mobile phase water phase, and the pH value of the water phase is set respectively 3.9 (adjusted with formic acid) and 7.2 (without pH regulator), the influence of different pH values ​​on levamisole was determined. Such as Figure 8 As shown, the peak symmetry is the best when the pH value is 3.9.

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Abstract

The invention discloses a fast extraction and LC-MS-MS detection method of benzimidazole and thiazole type residual medicine in an aquatic product. The method comprises the following steps that (1) muscle samples of the aquatic product are weighed; internal standard deuteratedalbendazole, deuterated mebendazole, magnesium sulfate, sodium chloride and acetonitrile are added for vortex extraction; (2) C18 powder and neutral alumina are added into extraction liquid; after swirling, nitrogen gas is used for blow-drying; filtering is performed after redissolution; (3) filter liquid is subjected to LC-MS-MS quantitative measurement; an internal standard method is used for calculating the residual quantity of levamisol, amino-mebendazole, hydroxyl-mebendazole, mebendazole, albendazole sulfoxide, albendazole sulphone, albendazole amino sulfone and albendazole. The method has the advantages that the sample treatment is simple, convenient and fast; meanwhile, the pH value of a liquid chromatography water phase and a cleaning agent is preferentially selected; the residual quantity of various benzimidazole and thiazole type medicines in the aquatic product can be simultaneously measured; the sensitivity is high; the repeatability is good; the accuracy is high; the lowest quantification of the medicine detection can reach 1mu g/kg.

Description

technical field [0001] The invention belongs to the field of quality and safety of aquatic products, and in particular relates to a rapid extraction method of benzimidazole and thiazole residues in aquatic products and a LC-MS-MS detection method. Background technique [0002] With the expansion of aquaculture scale, large-scale parasitic diseases continue to occur, and a large number of insecticides are applied to aquaculture. Significant drug residues were caused by off-label use and non-compliance with withdrawal periods. Most antiparasitic drugs have certain toxicity. For example, clinical trials have shown that most benzimidazole drugs have teratogenic and mutagenic effects. Serious adverse reactions have also occurred during the use of such drugs, such as anaphylactic shock, severe measles and encephalitis syndrome, which have attracted widespread attention from various countries. In 2004, my country's Adverse Drug Reaction Monitoring Center reported for the first ti...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N30/06G01N30/88G01N30/86
CPCG01N30/06G01N30/8634G01N30/88
Inventor 胥宁艾晓辉董靖刘永涛杨移斌杨秋红
Owner YANGTZE RIVER FISHERIES RES INST CHINESE ACAD OF FISHERY SCI
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