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LC-MS/MS determination method for residual quantity of rimantadine in egg

An LC-MS, rimantadine technology, applied in the field of determination of veterinary drug residues in eggs, to avoid matrix interference, good repeatability and high sensitivity

Inactive Publication Date: 2021-02-05
武汉工控检验检测有限公司 +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0013] In summary, liquid chromatography-tandem mass spectrometry has the advantages of efficient separation, multi-component qualitative and quantitative, etc., but the current detection of rimantadine residues mostly involves chicken, tissue and feed, and is used to detect the residues of rimantadine in eggs. There are few HPLC-MS / MS methods. The Ministry of Agriculture and Rural Affairs Announcement No. 197 formulated in 2019 established a liquid chromatography-tandem mass spectrometry method for the determination of 7 antiviral drugs such as ribavirin, but only involves feed

Method used

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  • LC-MS/MS determination method for residual quantity of rimantadine in egg
  • LC-MS/MS determination method for residual quantity of rimantadine in egg
  • LC-MS/MS determination method for residual quantity of rimantadine in egg

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0054] Example 1: Detection of rimantadine residues in eggs

[0055] (1) extraction

[0056] Take the eggs to be tested, break them, stir the egg yolks and egg whites evenly with a homogenizer, weigh 2±0.02g samples into a 50mL centrifuge tube, add 100μL of 20μg / L internal standard, mix well, let stand for 30min, add 1% Acetic acid acetonitrile solution 10mL, vortex 2min, centrifuge at 10000r / min for 5min, transfer the supernatant to a 50mL centrifuge tube, repeat the extraction once, combine the supernatant twice, add n-hexane 15mL, vortex 1min, 10000r / min Centrifuge for 10 min, discard the n-hexane layer, and set aside.

[0057] (2) purification

[0058] Mixed cation solid-phase extraction column Oasis MCX was activated with 3mL methanol, equilibrated with 3mL water, then the supernatant was put on the column, the flow rate was controlled at 2-3 drops / s, rinsed with 3mL 2% hydrochloric acid aqueous solution, 3mL methanol, and drained 3min, eluted with 5mL 5% ammonia water...

Embodiment 2

[0088] Example 2 Determination method

[0089] The qualitative determination is qualitative by comparing the retention time of the sample chromatogram with the retention time of the standard, and the characteristic ions of the chromatographic peak and the characteristic ions of the chromatographic peak of the corresponding concentration standard. The relative deviation of the retention time between the sample and the standard is not more than 2.5%; the relative abundance of the characteristic ion of the sample is consistent with the relative abundance of the standard solution with equivalent concentration, and the relative abundance deviation does not exceed the provisions in Table 3, then it can be judged that there is corresponding measured object. The deviation of the retention time is within ±5%, and the relative abundance of the detected ions should be consistent with the relative abundance of the calibration standard solution with equivalent concentration. Its allowable...

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Abstract

The invention discloses an LCMS / MS determination method for the residual quantity of rimantadine in an egg. The method comprises the following steps: extracting and purifying an egg sample, preparinga standard solution, determining the sample and the like. A sample pretreatment method which is simple, convenient, rapid and capable of effectively avoiding matrix interference in a sample is established, the pretreatment method is combined with LCMS / MS to be applied to qualitative confirmation and quantitative detection of rimantadine in the egg, the average recovery rate is 87.43%-96.74%, the average relative standard deviation (RSD) is 0.12%-0.45% (intra-batch) and 0.04%-0.23% (inter-batch), the detection limit is 0.3 [mu]g / kg, and the limit of quantitation is 1 [mu]g / k. The method has theadvantages of simplicity and convenience in operation, quickness, accuracy, high sensitivity and good repeatability.

Description

technical field [0001] The invention relates to a method for determining residual veterinary drugs in eggs, more specifically, a method for qualitatively and quantitatively determining residual rimantadine in eggs by using liquid chromatography-tandem mass spectrometry (LC-MS / MS), and belongs to the field of detection of residual veterinary drugs . Background technique [0002] Eggs contain high protein content and amino acids in a suitable ratio. They have high nutritional value and are easily absorbed by the human body, so they are widely loved by people. As the world's largest producer of eggs, my country has a great demand for eggs. However, in recent years, the problem of excessive drug residues in eggs has occurred frequently. Therefore, the quality and safety of eggs cannot be ignored. [0003] Rimantadine is one of the earliest drugs used to inhibit influenza virus. It has a good effect on the prevention and treatment of influenza, and has been widely used in the pr...

Claims

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Application Information

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IPC IPC(8): G01N30/02G01N30/06G01N30/14
CPCG01N30/02G01N30/06G01N30/14
Inventor 张美朱莉莎徐飘飘曾婧向文婷袁园园彭大鹏
Owner 武汉工控检验检测有限公司
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