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Method for detecting aminoglycosides in milk

An aminoglycoside and detection method technology, which is applied to the detection field of aminoglycosides in milk, can solve the problems of mass spectrometry pollution, cannot detect 11 kinds of aminoglycosides in milk at the same time, etc., and achieves good separation effect and saves reagents. Consumption and time spent in pretreatment, overcoming poor retention and separation

Inactive Publication Date: 2019-04-09
上海市农产品质量安全检测中心
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Problems solved by technology

[0007] The technical problem to be solved by the present invention is to provide a detection method for aminoglycosides in milk, which overcomes the fact that the prior art cannot detect 11 kinds of aminoglycosides in milk at the same time, and the use of ion-pairing reagents in the detection process pollutes the mass spectrometer Defects

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  • Method for detecting aminoglycosides in milk
  • Method for detecting aminoglycosides in milk
  • Method for detecting aminoglycosides in milk

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Embodiment 1

[0040] 1. Reagents and materials

[0041] 1.1 The experimental water should meet the first-class water specified in GB / T 6682.

[0042] 1.2 Acetonitrile: chromatographically pure (Merke, Germany).

[0043] 1.3 Methanol: chromatographically pure (Merke, Germany).

[0044] 1.4 Formic acid: chromatographically pure (CNW, Germany).

[0045] 1.5 Trichloroacetic acid: analytically pure (Jiangsu Yonghua Chemical Technology Co., Ltd.).

[0046] 1.6 Ammonia water: analytically pure (Sinopharm Chemical Reagent Co., Ltd.).

[0047] 1.7 Ammonium acetate: chromatographically pure (CNW, Germany).

[0048] 1.8 Potassium dihydrogen phosphate: analytically pure (Merke, Germany).

[0049] 1.9 Heptafluorobutyric acid (German CNW, purity ≥ 98.0%).

[0050] 1.10 50mM Potassium Dihydrogen Phosphate Solution (pH 7.0-8.0): Accurately weigh 0.68g Potassium Dihydrogen Phosphate, add water to dissolve to 100mL, adjust pH to 7.0-8.0 with ammonia water.

[0051] 1.11 Eluent: Accurately measure 400 ...

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Abstract

The invention relates to a method for detecting aminoglycosides in milk, which comprises the following steps: (1) extracting; (2) preparing a standard working solution; (3) performing determination bya high performance liquid chromatography-tandem mass spectrometry (HPLC-MS / MS), wherein the aminoglycosides are paromomycin, tobramycin, gentamicin, kanamycin, amikacin, apramycin, streptomycin, dihydrostreptomycin, neomycin, spectinomycin and hygromycin B. An MIP solid phase extraction column is uses in the step of extracting, thereby simplifying the pretreatment step, reducing the consumption of reagents and the time uses for the pretreatment; a SiELC Obelisc R chromatographic column is used for the separation of 11 kinds of aminoglycosides; and the mobile phase does not require heptafluorobutyric acid and does not contaminate the mass spectrometry.

Description

technical field [0001] The invention belongs to the technical field of detection of aminoglycoside drug residues in milk, and in particular relates to a method for detecting aminoglycoside drug residues in milk. Background technique [0002] Milk has become a daily necessity for human beings and has high nutritional value. The types of minerals in milk are also very rich. In addition to the well-known calcium, the content of phosphorus, iron, zinc, copper, manganese, and molybdenum is very high. [0003] Aminoglycoside antibiotics are a class of alkaline antibiotics with strong water solubility, which are extracted from the culture solution of Streptomyces or Micromonospora or semi-synthesized from natural products. It has a bactericidal effect in the stationary phase, and has a good inhibitory effect on both Gram-negative and positive bacteria. It belongs to a broad-spectrum antibiotic. Due to its high efficiency and low price, it is widely used in the breeding industry, ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N30/02
CPCG01N30/02G01N2030/027
Inventor 王敏汪弘康周雨璊
Owner 上海市农产品质量安全检测中心
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