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A multiple detection method for amantadine, rimantadine, ribavirin, and morpholinidine residues in poultry eggs

A technology of amantadine and rimantadine, which is applied to the residues of ribavirin and morpholine guanidine, and the field of multiplex determination of amantadine and rimantadine in eggs, which can solve the problem of inconsistency and reduce LC-MS/MS. Matrix effect, complex operation process and other problems, to achieve the effect of high accuracy, elimination of internal and external material interference, and short analysis time

Active Publication Date: 2017-03-01
山东世通检测评价技术服务有限公司
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Problems solved by technology

Both GC and GC-MS require a complex derivatization process before detection, and the operation process is relatively complicated, while LC-MS / MS with high selectivity and high sensitivity has certain advantages in the detection of antiviral drug compounds. However, better pretreatment methods are still needed to reduce the matrix effect of LC-MS / MS, especially for complex animal tissue samples, which have certain limitations
[0004] Chinese patent (CN201210228633.9) discloses an analysis method for the detection of diazepam and its metabolites in human urine samples by LC-MS / MS method, which can only detect a single drug and metabolites, and the pretreatment method is also different from that of The processing of animal tissue samples is very different. Therefore, a sample preparation method that can reduce the matrix effect of LC-MS / MS and an effective method for separating target compounds for qualitative and quantitative determination is urgently needed.

Method used

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  • A multiple detection method for amantadine, rimantadine, ribavirin, and morpholinidine residues in poultry eggs
  • A multiple detection method for amantadine, rimantadine, ribavirin, and morpholinidine residues in poultry eggs
  • A multiple detection method for amantadine, rimantadine, ribavirin, and morpholinidine residues in poultry eggs

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Embodiment 1

[0039] (1) The main equipment and materials used in this example:

[0040] Ultra-high performance liquid chromatography tandem mass spectrometer (Agilent, model 1260-6460); ultra-high speed centrifuge (Hitachi, model CR22GIII).

[0041] Aqueous microporous membrane (Adjar Technology, 0.22 μm); cation exchange solid-phase extraction column (Adjar Technology, Cleanert PCX, 60mg / 3ml).

[0042] (2) Sample processing steps:

[0043]Extraction: Take 3 egg samples, remove the shell, break the egg white and yolk, homogenize, measure 2mL and transfer it to a 50ml centrifuge tube, place it in a low temperature environment of -26°C for 2 hours, take it out and put it in a 50°C water bath 0.5h, repeated freezing and thawing twice, cooled to room temperature, added 10ml of methanol-1% formic acid solution (1:1, v / v), vortexed for 5min, oscillated horizontally for 2min, centrifuged at 10000r / min for 15min at room temperature, Take the supernatant, wash the residue with methanol-1% formic ...

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Abstract

The invention belongs to the technical field of poultry product detection and relates to a combined detection method of amantadine, rimantadine, ribavirin and moroxydine residues in eggs. The method comprises the following steps: carrying out low temperature repetitive freeze-thawing on a sample, adding a formic acid-methanol solution, mixing, centrifuging, taking a supernatant for standby, adding water saturated n-hexane, mixing, carrying out ultrasonic treatment, centrifuging to remove n-hexane floccules on the upper layer with an extracting solution left at the lower layer, purifying with a cation exchange solid-phase extraction column, measuring by a liquid chromatography-tandem mass spectrometer provided with an ESI source, and carrying out accurate qualitative and quantitative analysis on residues of the four antiviral drugs in eggs. The method provided by the invention has high specificity, can accurately and simultaneously measure residual quantity of amantadine, rimantadine, ribavirin and moroxydine without pollution, has high sensitivity, and provides technical support for guaranteeing quality safety of eggs.

Description

technical field [0001] The invention belongs to the technical field of poultry product detection, and relates to a non-polluting, high-efficiency multiplex method for determining amantadine, rimantadine, ribavirin and morpholinidine residues in poultry eggs. Background technique [0002] Since the 1960s, more than 20 antiviral drugs have been developed and marketed by human beings. Among them, four drugs, such as amantadine, rimantadine, ribavirin, and morpholinoguanidine, have a certain inhibitory effect on influenza virus. They are transplanted for veterinary use. Although they have a certain inhibitory effect on viruses such as avian influenza, they lack scientific norms and experimental data on safety and effectiveness. If these drugs are used in large quantities for a long time, it will lead to problems such as animal poisoning, immunosuppression, and drug residues. At the same time, it can also cause the virus to mutate, which will eventually cause great harm to human ...

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): G01N30/88
Inventor 孙海新许娜张慧孙丕春黄金发
Owner 山东世通检测评价技术服务有限公司
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