Determination method of polymyxins E residue content in animal source food by superhigh liquid chromatogram-tandom mass spectrometry

A technology of ultra-high liquid chromatography and polymyxin, which is applied in the field of determination of polymyxin E residues, can solve problems such as high toxicity, and achieve the effect of convenient method, easy implementation, and reliable implementation

Inactive Publication Date: 2011-11-02
谱尼测试集团深圳有限公司
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

The main veterinary clinical applications are polymyxin B and polymyxin E, among whic...

Method used

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  • Determination method of polymyxins E residue content in animal source food by superhigh liquid chromatogram-tandom mass spectrometry
  • Determination method of polymyxins E residue content in animal source food by superhigh liquid chromatogram-tandom mass spectrometry
  • Determination method of polymyxins E residue content in animal source food by superhigh liquid chromatogram-tandom mass spectrometry

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0039] Example 1, the precision and recovery detection of polymyxin E residues in chicken:

[0040] Weigh 5.0012g (accurate to 0.0001g) of the pulverized sample into a 50mL stoppered centrifuge tube, add 25mL of extraction solution, homogenize for 2min, and centrifuge at 4°C for 10min. Transfer the supernatant to another centrifuge tube, add 20mL extraction solution to the residue and repeat the above extraction operation. After combining the two extracted supernatants, add 20 mL of n-hexane to vortex for 2 min, centrifuge for 10 min, and discard the supernatant. Add 20 mL of n-hexane to the lower layer to repeat the above degreasing operation, and the obtained lower layer is to be purified.

[0041] The sample extract obtained above was transferred to the Oasis HLB purification column (pre-washed and activated with 6 mL each of methanol and water), washed with 10 mL of water first, and the effluent was discarded. Then eluted with 3 mL of methanol, collected the eluate, and ...

Embodiment 2

[0069] Embodiment 2, detection of polymyxin E precision and recovery rate in pig liver:

[0070] Weigh 5.0210g (accurate to 0.0001g) of the pulverized sample into a 50mL stoppered centrifuge tube, add 25mL of extraction solution, homogenize for 2min, and centrifuge at 4°C for 10min. Transfer the supernatant to another centrifuge tube, add 20mL extraction solution to the residue and repeat the above extraction operation. After combining the two extracted supernatants, add 20 mL of n-hexane to vortex for 2 min, centrifuge for 10 min, and discard the supernatant. Add 20 mL of n-hexane to the lower layer to repeat the above degreasing operation, and the obtained lower layer is left for purification.

[0071] The sample extract obtained above was transferred to the Oasis HLB purification column (pre-washed and activated with 6 mL each of methanol and water), washed with 10 mL of water first, and the effluent was discarded. Then eluted with 3 mL of methanol, collected the eluate, ...

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Abstract

The invention relates to a determination method of polymyxins E residue content in animal source food by superhigh liquid chromatogram-tandom mass spectrometry. The method comprises the following steps: adding an extract in a sample to be measured, fully whirling and extracting, high-speed freezing and centrifuging, then obtaining a sample liquid after filtering and purifying; weighing a polymyxins E standard sample, dissolving by methanol to take it as a storing solution, then further, diluting by methanol to obtain a standard working solution possessing a concentration gradient; detecting the sample by using a superhigh liquid chromatogram-tandom quadrupole liquid chromatography-mass spectrometer; reading out the concentration value of polymyxins E on a standard curve, and calculating the result of polymyxins E of the sample. According to the invention, the determination method of polymyxins E residue in animal source food is rapid and effective, the relative average deviation is less than 10%. Therefore, the method provided in the invention is reliable and easy to enforce for detecting polymyxins E residue in animal source food, which is capable of satisfying the requirments of research and production.

Description

[0001] Determination method of polymyxin E residue technical field [0002] The invention relates to a method for determining the residual amount of polymyxin E in animal-derived foods, in particular to a method for detecting the residual amount of polymyxin E in animal-derived foods by using an ultra-high performance liquid chromatography-tandem mass spectrometer Methods. Background technique [0003] Polymyxin belongs to the class of polypeptide antibiotics and mainly has five components: A, B, C, D, and E. Veterinary clinical applications are mainly polymyxin B and polymyxin E, among which polymyxin B has the strongest antibacterial activity, but its toxicity is relatively high. Polymyxin E, colistin, has low toxicity and good antibacterial activity. Polymyxin E is a basic polypeptide antibiotic produced by Koyama et al. from the soil of Fukushima Prefecture and isolated from the culture medium of a strain of Bacillus polymyxa antienemy. Polymyxin E, also known as coli...

Claims

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Application Information

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IPC IPC(8): G01N30/06G01N30/36G01N30/72
Inventor 宋薇
Owner 谱尼测试集团深圳有限公司
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