Method for detecting chloramphenicol residual in functional food through HPLC-MS-MS

A technology of HPLC-MS-MS and detection method, which is applied in the field of detection of chloramphenicol residues in functional foods, can solve the problems of chloramphenicol residue detection that has not been reported in the literature, difficulty in detecting chloramphenicol residues, and high mortality , to achieve the effect of overcoming sample matrix interference, good accuracy and high sensitivity

Active Publication Date: 2013-06-26
TIANJIN TIANSHI BIOLOGICAL DEV +2
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Problems solved by technology

The second is irreversible aplastic anemia, which is rare but has a high mortality rate. This reaction is an allergic reaction and has no direct relationship with the dosage and course of treatment.
The ingredients in functional foods are relatively complex, and most of them contain a variety of different ingredients, which makes it difficult to detect chloramphenicol residues in them
At present, there is no literature report on the detection of chloramphenicol residues in functional foods

Method used

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  • Method for detecting chloramphenicol residual in functional food through HPLC-MS-MS
  • Method for detecting chloramphenicol residual in functional food through HPLC-MS-MS
  • Method for detecting chloramphenicol residual in functional food through HPLC-MS-MS

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Embodiment 1

[0038] A kind of HPLC-MS-MS detection method of chloramphenicol residue in functional food, comprises the following steps: (take the nutrient high calcium granule as sample to be tested)

[0039] (1) Weigh 1g of high calcium granule as the sample, accurate to 0.01g, put it in a 50mL polypropylene centrifuge tube, add 15μL of deuterated chloramphenicol with a concentration of 0.4μg / mL as the internal standard solution, add 15mL of ethyl acetate Ester 0.45mL ammonium hydroxide, 5g anhydrous sodium sulfate, homogeneously extract for 30s, centrifuge at 4000r / min for 5min, transfer the supernatant to a 100mL chicken heart bottle;

[0040] (2) Take the second 50mL centrifuge tube, add 15mL ethyl acetate and 0.45mL ammonium hydroxide as the washing solution, wash step (1) using the knife head for homogenization operation for 10 seconds, and transfer the washing solution into the 100mL chicken heart bottle , then add 15mL ethyl acetate and 0.45mL ammonium hydroxide to the second 50mL ...

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Abstract

The invention discloses a method for detecting chloramphenicol residual in a functional food through HPLC-MS-MS. The method comprises the following steps: weighing a sample, adding deuterated chloramphenicol as an internal standard solution, adding ethyl acetate, ammonium hydroxide and anhydrous sodium sulfate, homogeneously extracting, centrifuging, and transferring the obtained supernatant to a heart-shaped bottle; concentrating the supernatant in the heart-shaped bottle to dryness; dissolving with water, carrying out ultrasonic treatment, adding n-hexane, carrying out vortex mixing, allowing the obtained solution to stand for layering, discarding n-hexane which is the upper layer, adding n-hexane, carrying out vortex mixing, allowing the obtained solution to stand for layering, transferring the obtained water phase to a centrifuge tube, centrifuging, and allowing the centrifuged water phase to go through a filter membrane to obtain a final solution for the determination through HPLC-MS-MS; accurately weighing a chloramphenicol standard substance, carrying out ultrasonic dissolving with chromatographically pure methanol, adding the chromatographically pure methanol to a constant volume, and preparing chloramphenicol standard substance solutions having different concentrations; determining the chloramphenicol standard substance solutions through the HPLC-MS-MS to obtain a standard curve; and calculating according to obtained examination data through the standard curve to obtain the concentration of chloramphenicol in the sample to be measured. The method has the advantages of good accuracy, high precision and good linearity.

Description

technical field [0001] The invention relates to a detection method for chloramphenicol residue in functional food. technical background [0002] Since the reform and opening up, the functional food industry, as a sunrise industry in the 21st century, has shown more and more vitality. Functional foods have also gradually entered the lives of the broad masses of the people. played an important role. [0003] The production and preparation of animal-derived functional foods such as calcium powder, milk powder, protein powder and honey are mostly based on animal husbandry, aquatic animal products and semi-finished products, and chloramphenicol has inhibitory effects on both Gram-positive and negative bacteria , and has a strong effect on the latter, among which the effect on typhoid bacillus, influenza bacillus, parainfluenza bacillus and pertussis bacillus is stronger than other antibiotics, and it is also effective against rickettsial infections such as typhus, so it is widel...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N30/88
Inventor 赵晓娟李星芝王俊全
Owner TIANJIN TIANSHI BIOLOGICAL DEV
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