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A method for analyzing residual veterinary drugs in mutton

A technology for mutton and veterinary drugs, applied in analytical materials, material separation, instruments, etc., can solve the problems of high detection limit and quantification limit, high cost, affecting test results, etc., and achieve high accuracy and purification effect. and low limits of quantitation, high sensitivity and precision

Active Publication Date: 2020-10-09
XINJIANG ACADEMY OF ANIMAL SCI QUALITY STANDARDS INST OF ANIMAL HUSBANDRY XINJIANG UYGUR AUTONOMOUS REGION SHEEP & WOOL CASHMERE QUALITY SAFETY SUPERVISION & INSPECTION CENT
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Problems solved by technology

In addition, streptomycin can damage the baby's auditory nerve, causing hearing impairment in newborns
Certain benzimidazole veterinary drugs may cause mutations in human cells
Third, due to the long-term exposure of animals to antibacterial drugs, they accumulate in the body, and the drug-resistant microorganisms in the animal body are selectively multiplied, which reduces the efficacy of some commonly used drugs, such as penicillin, chloramphenicol, and gentamicin. , sulfonamides and other drugs have developed resistance in livestock production
In order to prohibit the excessive use of veterinary drugs in animal husbandry, many countries and international organizations, including China, have set strict limits on the residues of veterinary drugs in meat such as cattle, sheep, pigs, and horses, including "tentative maximum residues". ", "All limited standards", "Exempted eggs", etc., but there are still many problems in the detection of these veterinary drugs
[0004] The current veterinary drug detection methods in my country are mainly based on the classification of veterinary drugs. These methods have exposed several defects: for example, the screening ability for non-testing items of veterinary drug residues is insufficient, and for different types of veterinary drug residues, its detection method There are differences, so that the detection of veterinary drug residues can only measure the specified types of veterinary drugs, but lacks the ability to screen for other types of non-detected veterinary drug residues in the sample, which makes food safety monitoring hidden dangers
Secondly, different pretreatment and detection methods are required for different veterinary drug residue detection items of the same sample, which not only prolongs the detection cycle, increases detection cost and difficulty, but also reduces work efficiency
Furthermore, the extraction and purification process of traditional veterinary drug detection methods is cumbersome, costly, and time-consuming, which is difficult to meet the purpose of large-scale sample determination
Moreover, when detecting the content of residual veterinary drugs in meat, due to the relatively strong interaction between some veterinary drugs and the meat matrix, the detection process has a greater impact on the detection of some veterinary drugs, resulting in deviations in the detection limit and quantitative limit of these drugs. High, for example, salbutamol in mutton, due to its special structure, is affected by the mutton matrix and solvent during the detection process, the detected result is lower than its actual content, and may affect the test results of other veterinary drugs

Method used

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  • A method for analyzing residual veterinary drugs in mutton

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0081] Embodiment 1 provides a kind of method for analyzing residual veterinary drug in mutton, comprises the steps:

[0082] (1) mince the mutton sample and homogenize it in a homogenizer;

[0083] (2) Weigh 5.00g of homogenized mutton sample into a 50ml centrifuge tube, add 10ml of 0.2mol / L sodium acetate buffer solution, and add acetic acid to adjust the pH value to 5, mix well; then add 0.1ml of the same amount of β-glucuronidase and arylsulfatase, shake and mix well, then hydrolyze in a constant temperature water bath at 35°C for 12 hours, centrifuge at 4000 rpm for 5min, transfer the separated supernatant to a 50ml centrifuge tube; centrifuge Add 5ml of formic acid to the final residue, vortex on a vortex mixer for 2min, centrifuge at 4000 rpm for 5min, and combine with the obtained supernatant;

[0084] (3) Add perchloric acid to the obtained supernatant to adjust the pH value to 0.5, mix evenly for 10 minutes, then concentrate the obtained supernatant after centrifugi...

Embodiment 2

[0111] Embodiment 2 provides a kind of method for analyzing residual veterinary drug in mutton, comprises the steps:

[0112] (1) mince the mutton sample and homogenize it in a homogenizer;

[0113] (2) Weigh 5.00g of homogenized mutton sample into a 50ml centrifuge tube, add 10ml of 0.2mol / L sodium acetate buffer solution, and add acetic acid to adjust the pH value to 5.2, mix well; then add 0.1ml of the same amount of For β-glucuronidase and arylsulfatase, oscillate and mix evenly, then hydrolyze in a constant temperature water bath at 37°C for 24 hours, centrifuge at 4000 rpm for 5min, and transfer the separated supernatant to a 50ml centrifuge tube; centrifuge Add 5ml of formic acid to the final residue, vortex on a vortex mixer for 2min, centrifuge at 4000 rpm for 5min, and combine with the obtained supernatant;

[0114] (3) Add perchloric acid to the obtained supernatant to adjust the pH value to 1.2, mix evenly for 15 minutes, then concentrate the obtained supernatant ...

Embodiment 3

[0139] Embodiment 3 provides a kind of method for analyzing residual veterinary drug in mutton, and difference with embodiment 2 is that the extraction agent extraction process described in the (4) step adopts gradient extraction method, comprises the following steps;

[0140] A) To adjust the pH value to 11, and add salting-out agent centrifugation, add 10ml equivalent formic acid and dimethyl sulfoxide to the supernatant, homogenize for 30min, centrifuge, filter to get the supernatant; for centrifugation The resulting sample residue was extracted 3 times according to this procedure, and the obtained supernatants were combined and blended to obtain X 1 Extraction solution;

[0141] B) The X obtained in step A 1 Concentrate the extract and transfer it to a 50ml centrifuge tube, add 10ml of acetonitrile, homogenize for 30min, centrifuge, filter to get the supernatant; repeat the extraction of the sample residue obtained by centrifugation three times according to this step, and...

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Abstract

The invention relates to the field of analysis and testing and particularly relates to a method for analyzing residual veterinary drugs in mutton. The method at least comprises sample pretreatment, enzymatic hydrolysis, extraction, purification and on-machine testing. Compared with the existing detection method, the method provided by the invention has higher accuracy, extracts, purifies and testsa variety of veterinary drugs, and is fast and efficient. The method utilizes a multi-extraction method using three different solvents, fully extracts the veterinary drugs in mutton as many as possible, improves the detection accuracy and reduces the influence caused by the base on the veterinary drugs. In gradient elution, three mobile phases are used so that it is solved that the original two mobile phases with solubility under action of an adsorbent in a chromatographic column are layered so that the target drugs are respectively dissolved in two solvents, the characteristic peak detectedby the detector splits into a primary characteristic peak and a secondary characteristic peak, the drug content capable of being detected is reduced and the determination of other drugs is influenced.

Description

technical field [0001] The invention relates to the field of detection and analysis of veterinary drugs, in particular to a method for analyzing residual veterinary drugs in mutton. Background technique [0002] Nowadays, the use of veterinary drugs is inevitable in animal husbandry production. In order to ensure food safety, my country has established a corresponding withdrawal period system for veterinary drugs. Withdrawal period for veterinary drug residues refers to the interval between the cessation of dosing of livestock and poultry and the approval of slaughter or the approval of their products on the market. Announcement No. 278 of the Ministry of Agriculture of the People's Republic of my country stipulates that all drugs or other chemical substances used for food animals must have a drug withdrawal period. However, in the actual animal husbandry process, due to the lack of relevant knowledge and the drive of economic interests, some livestock farmers failed to imp...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): G01N30/02G01N30/06
CPCG01N30/02G01N30/06G01N2030/047
Inventor 胡波高维明宫平魏佩玲周卫东吕雪峰
Owner XINJIANG ACADEMY OF ANIMAL SCI QUALITY STANDARDS INST OF ANIMAL HUSBANDRY XINJIANG UYGUR AUTONOMOUS REGION SHEEP & WOOL CASHMERE QUALITY SAFETY SUPERVISION & INSPECTION CENT
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