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Method for detecting residues of chloramphenicols in milk products

A detection method, the technology of chloramphenicol, applied in measuring devices, instruments, and material analysis through electromagnetic means, etc., can solve problems such as unavoidable emulsification of ethyl acetate, inaccurate detection, incomplete extraction of chloramphenicol, etc.

Active Publication Date: 2016-03-30
INNER MONGOLIA MENGNIU DAIRY IND (GRP) CO LTD +1
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  • Abstract
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Problems solved by technology

[0004] At present, these methods cannot avoid the emulsification phenomenon produced in the ethyl acetate extraction process, which will make the extraction of chloramphenicol incomplete. At present, the internal standard method is generally used to avoid the inaccurate detection caused by this problem, but due to the internal standard The material is expensive, and the cost of testing a single sample will be higher

Method used

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  • Method for detecting residues of chloramphenicols in milk products
  • Method for detecting residues of chloramphenicols in milk products
  • Method for detecting residues of chloramphenicols in milk products

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Embodiment

[0028] 1. General method:

[0029] 1 sample processing

[0030] 1.1 Raw milk, fermented milk, sterilized milk, modified milk, pasteurized milk, milk beverages and other liquid dairy products

[0031] Weigh about 5.0 g of the sample (accurate to 0.01 g), add 15 mL of ethyl acetate, vortex for 1 min, then sonicate for 20 min, centrifuge at 10000 r / min for 10 min, take 7.5 mL of the supernatant and put it in a test tube, and store it at 40 °C ± Blow dry with nitrogen at 2°C. Dissolve in 0.5mL methanol, dilute with 5mL ultrapure water, vortex mix, then add 5mL n-hexane, vortex mix, centrifuge at 3000r / min for 2min, discard the upper layer of n-hexane, and extract the lower layer through HLB solid phase extraction Small column (activated with 3mL methanol and 3mL ultrapure water in advance), remove impurities with 5mL water when it dries quickly, and then dry it with a vacuum pump (or blow dry with an ear ball), add 6mL methanol to elute, and then use nitrogen gas 40 Blow dry at...

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Abstract

The invention discloses a method for detecting residues of chloramphenicols in milk products. Chloramphenicols include chloramphenicol, thiamphenicol and florfenicol. The method comprises the following steps: carrying out pretreatment on a to-be-detected sample: weighing m1g of the to-be-detected sample, adding v1ml of ethyl acetate for extraction to obtain a first extract, dissolving the first extract by virtue of v2ml of methanol, adding v3ml of normal hexane, mixing uniformly, carrying out centrifuging, abandoning superstratum to obtain a second extract, and purifying the second extract by virtue of a solid phase extraction column, so as to obtain purified substances; analyzing the purified substances by virtue of a liquid phase-tandem mass spectrometer, and detecting the residues of the chloramphenicols in the to-be-detected sample, wherein m1 is less than or equal to 5, v1 is less than 20, v2 is less than 1, and v3 is less than 8. According to the method, an interior label is not required, so that an emulsification phenomenon in the detection process can be avoided, and the interference caused by a matrix to the detection can be reduced; chloramphenicol drugs can be simultaneously detected, the sensitivity and the recovery rate are high, the cost is saved, and the operation is easy.

Description

technical field [0001] The invention relates to the field of food detection, in particular to a method for detecting chloramphenicol residues in dairy products. Background technique [0002] Chloramphenicol, thiamphenicol, and florfenicol (fluthiamphenicol) are generally more effective against gram-negative bacteria than gram-positive bacteria. Chloramphenicol, thiamphenicol, and florfenicol (fluthiamphenicol) have a high therapeutic index in animals and were once commonly used antibiotics in veterinary clinics. The main toxic and side effects of chloramphenicol, thiamphenicol, and florfenicol (fluthiamphenicol) are inhibition of hematopoietic function and irreversible aplastic anemia. Humans and young animals are very sensitive to chloramphenicol, thiamphenicol, and florfenicol (fluthiamphenicol). The European Union, China and many countries have listed chloramphenicol, thiamphenicol, and florfenicol (fluthiamphenicol) as banned veterinary drugs for food animals, and pres...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N30/02G01N30/34G01N27/62
CPCG01N27/62G01N30/02G01N30/34G01N2030/027
Inventor 李照张雪峰崔向云徐向峰常建军宋晓东
Owner INNER MONGOLIA MENGNIU DAIRY IND (GRP) CO LTD
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