LC-MS/MS (Liquid Chromatography-Mass Spectrometry/Mass Spectrometry) determination method for residual quantity of amantadine in eggs

A LC-MS, amantadine technology, applied in the field of determination of veterinary drug residues in eggs, to achieve the effect of avoiding matrix interference, good repeatability, and easy operation

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A LC-MS, amantadine technology, applied in the field of determination of veterinary drug residues in eggs, to achieve the effect of avoiding matrix interference, good repeatability, and easy operation

CN112198255AInactive Publication Date: 2021-01-08武汉工控检验检测有限公司 +1

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Effect test

Embodiment 1

[0052] Example 1: Detection of amantadine residues in eggs

[0053] (1) extraction

[0054] 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.

[0055] (2) purification

[0056] Activate the mixed cation solid phase extraction column Oasis MCX with 3mL methanol, balance with 3mL water, then take the supernatant and put it on the column, the flow rate is controlled at 2-3 drops / s, rinse with 3mL 2% hydrochloric acid aqueous solution, 3mL methanol successively, pump Dry for 3min, elute with 5mL 5% a...

Embodiment 2

[0083] Example 2 Determination method

[0084] Qualitative determination: through the comparison of the retention time of the sample chromatogram with the retention time of the standard, 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 the A corresponding analyte exists. The retention time deviation 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 deviation should me...

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Abstract

The invention discloses an LCMS / MS (Liquid Chromatography Mass Spectrometry / Mass Spectrometry) determination method for the residual quantity of amantadine in eggs. The method comprises the steps of egg sample extraction, purification, standard substance solution preparation, sample determination and the like. A sample pretreatment method which is simple, convenient, rapid and capable of effectively avoiding matrix interference in the sample is established, the pretreatment method is combined with LCMS / MS to be applied to qualitative confirmation and quantitative detection of amantadine in eggs, the average recovery rate is 96.60%-100.19%, the average relative standard deviation (RSD) is 0.06%-0.16% (in-batch) and 0.03%-0.06% (between-batch), the detection limit is 0.3 [mu]g / kg, and the quantification limit is 1 [mu]g / kg. The method has the advantages 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 the residual amount of veterinary drugs in eggs, more specifically, a method for qualitatively and quantitatively determining the residual amantadine content 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] As a major producer and consumer of livestock and poultry products, China ranks among the top in the world in terms of livestock and poultry products produced and consumed every year. Among these livestock and poultry products, eggs are one of the most consumed livestock and poultry products. According to statistics, the per capita consumption of eggs in cities and towns in my country in 2018 was 10.8 kg. Therefore, the food safety of eggs is more and more widely concerned by people. [0003] One of the main factors affecting the safety of eggs is veterinary drug residues. ...

Claims

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Application Information

Patent Timeline

08 Jan 2021

Publication

CN112198255A

IPC: G01N30/02; G01N30/06

CPC: G01N30/02; G01N30/06; G01N2030/062

Inventors: 张美; 朱莉莎