Method for determination of malachite green, quinolones and sulfonamides in aquatic products

A technology of sulfonamides and quinolones, which is applied in the field of ecological environment safety, can solve the problems of time-consuming detection, high detection cost, low accuracy of quantitative results, and high instrument maintenance cost, and achieves shortened measurement time, low detection limit, The effect of stable recovery rate

Inactive Publication Date: 2019-08-16
农业部渔业环境及水产品质量监督检验测试中心(天津)
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Problems solved by technology

Based on the above detection techniques, the advantage of liquid chromatography is that it is quantitatively accurate, but the disadvantage is that it is easily interfered by impurities and has poor qualitative accuracy. The disadvantage is that the maintenance cost of the instrument is high, and the enzyme-linked immunoassay assay has the characteristics of high specificity, sensitivity and rapidity. It is generally used for rapid screening. The disadvantage is that the accuracy of quantitative results is low.
At present, with the increase of detection tasks, the existing standard method has a single detection index, time-consuming detection and high detection cost. In order to solve the above problems, integrating two or several single detection indicators into one detection method has become Topics of current research

Method used

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  • Method for determination of malachite green, quinolones and sulfonamides in aquatic products
  • Method for determination of malachite green, quinolones and sulfonamides in aquatic products
  • Method for determination of malachite green, quinolones and sulfonamides in aquatic products

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0090] Embodiment 1, the selection of parent ion, daughter ion

[0091] In this study, liquid chromatography-tandem mass spectrometry was used to analyze the colorless / colorless malachite green, quinolones and sulfonamides in aquatic products, and more fragment information could be obtained by selecting (ESI+) positive ion scanning method, which was characterized by molecular ion peaks[ M+H]+ and its secondary fragments were used to characterize the three types of compounds, and the strongest secondary fragments were used for quantification.

[0092] The hydroxyl functional groups in colorless / colorless malachite green, quinolones and sulfonamides can be positively charged, and the (ESI+) ionization mode can provide more fragment information than the (ESI+) positive ion mode, and the sensitivity is greatly improved, such as figure 1 shown. In this method, 0.5 μg / mL colorless malachite green, quinolones, sulfonamides and their internal standard solution are continuously inject...

Embodiment 2

[0094] Embodiment 2, sample pretreatment conditions

[0095] Sample pretreatment

[0096] The present invention is based on GB / T19857-2005 liquid quality determination of malachite green and crystal violet residues in aquatic products and Ministry of Agriculture Announcement No. 1077-1-2008 of 17 kinds of sulfonamides and 15 kinds of quinolones in aquatic products. Based on the determination, the two methods are further optimized and integrated, and the original two methods are integrated into a method that can carry out compound extraction and on-machine measurement at the same time.

[0097] 1. Weighing of samples

[0098] Weigh the frozen samples after they are completely and naturally thawed. Samples should be taken from four diagonal areas of the minced meat. Sampling should avoid carrying thawed water to ensure the uniformity of the minced meat when weighing and reduce the error caused by unmixed matrix.

[0099] 2. Extraction

[0100] Accurately weigh 5.00g (±0.01g) of...

Embodiment 3

[0105] Embodiment 3, determination of detection conditions of AB5500Q liquid mass spectrometer

[0106] According to the relevant provisions of CAC and EU Resolution No. 657 / 2002 / EEC, two pairs of ions can be selected for MRM monitoring to meet the detection requirements. At the same time, the selection of product ions mainly considers the parent ion and product ion according to the mass spectrum and structure of each compound. Characteristic selection, and the matrix interference is less in the actual sample analysis. After determining the molecular ions of various substances according to the above principles, the molecular ions of various compounds are respectively used as parent ions, and the product ions are selected for a full scan. , The two pairs of product ions with less interference are qualitative ions, and the strongest pair is quantitative ions. Finally, various mass spectrometry parameters are optimized in the positive ion mode of multiple reaction monitoring (MRM)...

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Abstract

The invention relates to a method for determining malachite green, quinolone and sulfonamide drugs in aquatic products. The method comprises the following steps: step 1, preparing samples; step 2, extracting to-be-detected samples to obtain to-be-processed samples; step 3, determining chromatographic conditions; step 4, determining mass spectrum conditions; step 5, drawing a standard working curve; step 6, determining sensitivity, accuracy and precision. With adoption of the method, malachite green, leucomalachite green, quinolone and sulfonamide drugs in an extracted and concentrated aquatic product substrate are determined simultaneously for the first time, the problems that time is consumed and detection cost is high due to traditional respective extraction are solved, ion response value is increased, sensitivity is enhanced, detection limit is low, the effects of being qualitative, quantitative, accurate, fast, efficient and sensitive are realized truly, and the method can be taken as a reliable detection means for the three drugs and is applicable to extraction and concentration of a batch of samples.

Description

technical field [0001] The invention belongs to the application of liquid mass spectrometry in analytical chemistry and the technical field of ecological environment safety, in particular to a method for simultaneously measuring malachite green, quinolones and sulfonamides in aquatic products by using liquid mass spectrometry. Background technique [0002] With the improvement of intensive breeding of aquatic animals and the continuous deterioration of the breeding environment, aquatic animal diseases present the characteristics of many types of diseases, wide coverage, and irregular onset time. In order to avoid economic losses caused by diseases, farmers use a large number of drugs In addition to the current situation that there is no special aquatic drug to replace it, the problem of drug residue is becoming more and more prominent, and the quality and safety of aquatic products has attracted great attention from the government and society. Because malachite green, quinol...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): G01N30/02
CPCG01N30/02
Inventor 陈永平李春青高丽娜时文博李连庆孙晓旺张素青王娟娟赵爽
Owner 农业部渔业环境及水产品质量监督检验测试中心(天津)
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