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Preparation method of chloramphenicol-containing fishmeal standard material

A standard substance, chloramphenicol technology, applied in the field of fish meal matrix standard substance preparation, can solve the problems of impact judgment, low throughput, high analysis cost, etc., and achieve the effect of easy promotion, good uniformity and stability, and simple operation

Inactive Publication Date: 2017-06-09
NAT INST OF METROLOGY CHINA
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, due to the characteristics of mass spectrometry detection, the sample pretreatment and purification process is complicated, mainly including chloramphenicol extraction, protein removal, impurity purification, concentration, filtration and other processes, which make the analysis cost high, low throughput, and more importantly, cumbersome. Complicated pretreatment process, condition control, matrix effect, etc. affect the reliability and accuracy of the detection results. The relative standard deviation (RSD) of the results of liquid chromatography-mass spectrometry or gas chromatography-mass spectrometry methods reported in the literature is generally Between 20% and 35%, it directly affects the judgment of the results near the limit value

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  • Preparation method of chloramphenicol-containing fishmeal standard material
  • Preparation method of chloramphenicol-containing fishmeal standard material
  • Preparation method of chloramphenicol-containing fishmeal standard material

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Embodiment Construction

[0024] Preferred embodiments of the present invention are described below, and it should be understood that the preferred embodiments described here are only used to illustrate and explain the present invention, and are not intended to limit the present invention.

[0025] In this embodiment, the raw material, that is, a fish sample containing chloramphenicol, needs to be obtained first.

[0026] Candidates for standard substances were obtained by means of feeding. When purchasing tilapia, ensure that the water used for feeding and the fish tank do not contain chloramphenicol. After two weeks of blank feeding, the preliminary detection confirms that the fish meat is a blank sample. Chloramphenicol was added to the water body according to a certain dose, and chloramphenicol was added repeatedly after changing the water body every week, and the animals were continuously raised for 6 weeks.

[0027] 1. Fish sample pretreatment:

[0028] (1) Take positive tilapia, remove fishbon...

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Abstract

The invention discloses a preparation method of a chloramphenicol-containing fishmeal standard material. The method is characterized in that the raw fishmeal polluted by chloramphenicol is obtained through simulating feeding; a sample is preprocessed and mixed with water by proper ratio; then the mixture is uniformly pulped; the freeze-dried fish is obtained by a freezing drying method; the freeze-dried fish is grinded, screened, uniformly mixed and irradiated to prepare the freeze-dried fishmeal which is high in uniformity; the uniformity is detected, the stability is monitored, and the standard material is assigned by high-accuracy measuring through a liquid chromatography-isotope dilution mass spectrometry. The trace chloramphenicol containing freeze-dried fishmeal is high in uniformity and stability and is applicable to the evaluation of method for analyzing the trace chloramphenicol residue in an aquatic product, the quality control in analyzing, and the assessment of lab ability; the standard material is applicable to calibrating of metering devices and evaluation of measurement methods.

Description

technical field [0001] The invention relates to a method for preparing a fish meal base standard substance containing trace amounts of chloramphenicol. The chloramphenicol standard substance in the fish meal is a measurement standard and is mainly used for calibrating measuring instruments and evaluating the accuracy of measurement methods. Background technique [0002] Chloramphenicol (chloramphenicol, CAP), scientific name D-threo-(-)-N-[α-(hydroxymethyl)-β-hydroxy-p-nitrophenylethyl]-2,2-dichloroacetamide , the molecular formula is C 11 h 12 Cl 2 N 2 o 5 , white acicular or slightly yellow-green acicular, long flaky crystal or crystalline powder, melting point 149-153°C, specific optical rotation 19.5°C, water solubility 2.5g / L. Soluble in water and methanol, ethanol, acetone, propylene glycol, etc. The CAS number is 56-75-7 and the molecular weight is 323.1294. chemical structure such as figure 1 shown. [0003] Chloramphenicol is a high-efficiency broad-spectru...

Claims

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Application Information

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IPC IPC(8): G01N1/28A61L2/08
CPCA61L2/081G01N1/28
Inventor 李秀琴张庆合阚莹李红梅郑思珩
Owner NAT INST OF METROLOGY CHINA
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