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A value determining method for a sulfonamide veterinary drug residual matrix reference material in pork

A standard substance and matrix technology, which is applied in the field of analysis and detection, can solve the problems that the recovery rate and relative standard deviation need to be further optimized, affect the relative recovery rate and relative standard deviation of the drug, and cannot meet the value requirements of the matrix standard material. Avoid uneven quality, reduce content, and avoid the effect of adsorption

Inactive Publication Date: 2018-12-04
SHANGHAI INST OF MEASUREMENT & TESTING TECH
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  • Application Information

AI Technical Summary

Problems solved by technology

[0004] Liquid chromatography-tandem mass spectrometry (LC-MS / MS) is currently the main confirmation method for the detection of sulfonamides. However, due to the high fat content and protein content in pork, the pretreatment process is cumbersome, which significantly affects the reliability of the determination results. sex and accuracy
The standard recovery of LC-MS / MS reported in the literature is generally 70%-110%, and the standard deviation of the results is generally 15%-30%, which cannot meet the fixed value requirements of the matrix standard substance ("ultra high performance liquid chromatography-tandem Determination of sulfa drug residues in pork by mass spectrometry", Yang Mei et al., "Journal of Food Safety and Quality Inspection", Vol. 8, pp. 3633-3638, 2017)
[0005] CN 101949898 A discloses a method for detecting residues of various basic drugs in animal-derived foods. The method is extracted by vortexing and mixing acetonitrile, isopropanol and citric acid buffer solution, and hydrophilic polystyrene-diethylene Benzene solid-phase extraction column and cation-exchange solid-phase extraction column purification and liquid chromatography-mass spectrometry to detect a variety of basic drugs such as β-receptor agonists and sulfonamides in pork, pig liver, eggs, shrimp, and milk , benzodiazepines, nitroimidazoles, benzimidazoles, and triphenylmethane residues, but this method did not remove the water in the extraction solvent, which significantly affected the relative recovery and relative standard deviation of the drug. The relative recovery rate is only 63.1%-109.0%, and the relative standard deviation is 1.6%-23.0%, which cannot meet the value requirements of the matrix standard substance
[0006] CN 102175784 A discloses a method for the simultaneous determination of 54 drug residues in pork by solid-phase extraction-liquid chromatography-mass spectrometry / mass spectrometry. 18 Solid phase extraction cartridge cleanup, liquid chromatography-mass spectrometry / mass spectrometry (LC-MS / MS) determination, isotope internal standard dilution internal standard method and external standard method for quantification, the recovery range is 21.1%-121%, relative standard deviation less than 19.8%, it can be used as a screening method for the simultaneous determination of 54 drug residues in pork including sulfonamides, nitroimidazoles, quinolones, macrolides, lincosamides and praziquantel. Recovery and relative standard deviation still need to be further optimized

Method used

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  • A value determining method for a sulfonamide veterinary drug residual matrix reference material in pork
  • A value determining method for a sulfonamide veterinary drug residual matrix reference material in pork
  • A value determining method for a sulfonamide veterinary drug residual matrix reference material in pork

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preparation example Construction

[0083] Preparation of blank pork: obtained from pigs fed without adding drugs from the farm;

[0084] Preparation of candidate matrix standard substances for sulfonamide veterinary drug residues in pork: Pigs raised without adding drugs were ordered from the farm, administered intravenously according to the pre-designed dosage, and positive samples were obtained.

Embodiment 1

[0085] The preparation of embodiment 1 standard working solution

[0086] Preparation of standard stock solution: Accurately weigh 10.0 mg (accurate to 0.1 mg) of sulfamethazine veterinary drug purity standard substance and sulfamethazine veterinary drug purity standard substance converted to 100% purity respectively, dissolve completely with methanol, transfer to 10 mL brown In a volumetric flask, dilute to the volume with methanol, shake well, and prepare a standard stock solution with a mass concentration of 1 mg / mL, and store it in a refrigerator at -20°C in the dark, with a validity period of 12 months; accurately weigh the isotope-labeled solution whose purity is converted to 100%. Sulfamethazine and isotope-labeled sulfadiazine each 1.0mg (accurate to 0.1mg), completely dissolved in methanol, transferred to a 10mL brown volumetric flask, distilled to volume with methanol, shaken well, and prepared to a mass concentration of 0.1mg / mL Isotope-labeled standard stock soluti...

Embodiment 2

[0089] Embodiment 2 matrix standard substance pretreatment

[0090] (1) Sample preparation: take the carcass muscle on both sides of the pig, cut into meat slices of appropriate size, grind 3 times with a meat grinder with an aperture of 5 mm, and manually mix well;

[0091](2) Extraction: Accurately weigh 3.00g (accurate to 0.01g) of pork and place it in a 50mL centrifuge tube, add 300μL isotope labeled standard mixed solution with a concentration of 1μg / mL, mix on a vortex mixer for 1min, add 20mL Acetonitrile, homogenate for 2 minutes, centrifuge at 9000r / min (4°C) for 2 minutes, pass the obtained supernatant through a 70g anhydrous sodium sulfate column (infiltrated with acetonitrile in advance) to remove the water, and transfer it to a 100mL chicken heart bottle, repeat the operation Three times, the obtained extract was dried by rotary evaporation in a 50°C water bath, and 3 mL of n-hexane-saturated mobile phase (acetonitrile-0.1% formic acid aqueous solution (5:95)) was...

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Abstract

A value determining method for a sulfonamide veterinary drug residual matrix reference material in pork is provided. The method includes a matrix reference material pretreatment step. The pretreatmentincludes (1) a step of extraction, namely adding an extracting solvent into a matrix reference material for target substance extraction, and allowing an obtained liquid supernatant to pass through ananhydrous sodium sulfate column to obtain an extract; and (2) a step of purification, namely a step of subjecting the extract obtained in the step (1) to water-bath rotary evaporation drying, addinga mobile phase to a constant volume to dissolve the extract; performing filtration through a liquid-liquid partition purification process and performing filtration to obtain the pretreated matrix reference material, wherein the anhydrous sodium sulfate column is infiltrated with acetonitrile in advance and the mobile phase is saturated with n-hexane in advance. The n-hexane-saturated mobile phaseis added to the extract of the sulfonamide veterinary drug residual matrix reference material to a certain volume, thus reducing distribution of sulfonamide drug in an extract liquid into an organic phase during liquid-liquid partition. The sulfonamide drug recovery rate is 95.7-104.8%, and the relative standard deviation is less than 5% (with n being 6).

Description

technical field [0001] The invention belongs to the technical field of analysis and detection, and relates to a value determination method for a matrix standard substance of sulfonamide veterinary drug residues in pork. Background technique [0002] Sulfonamide veterinary drugs are a general term for a class of antibacterial drugs with a sulfanilamide structure. They have the advantages of wide antibacterial spectrum, strong antibacterial ability, and low price. They are widely used in the prevention and treatment of infectious diseases in food-borne animals. However, long-term consumption of animal-derived foods containing sulfonamide veterinary drugs is likely to cause allergic reactions, affect the function of the urinary system, produce crystalluria, hematuria and other symptoms, destroy the ecological balance of the normal flora of the body, and cause adverse consequences such as bacterial resistance. Sulfa veterinary drugs are one of the veterinary drugs whose residues...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N30/02G01N30/06
CPCG01N30/02G01N30/06G01N2030/027
Inventor 李兰英闻艳丽李杰孟娇然刘刚梁文李妍王乐乐
Owner SHANGHAI INST OF MEASUREMENT & TESTING TECH
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