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A kind of detection method of residual amount of chloramphenicol

A detection method and residue technology, applied in the direction of measuring devices, instruments, scientific instruments, etc., can solve the problems of humidity sensitivity, harm, and impact measurement, and achieve the effect of low sensitivity

Active Publication Date: 2018-03-16
国检测试控股集团京诚检测有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, BSTFA is very sensitive to the humidity of the environment, and the reaction conditions need to be strictly controlled, and the derivatized nitrogen-silicon bond and oxygen-silicon bond may decompose in the heating environment of the gas phase, affecting the determination
Pyridine is a poisonous gas with a foul smell. Using pyridine as a catalyst will cause secondary pollution and harm to experimenters.

Method used

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  • A kind of detection method of residual amount of chloramphenicol
  • A kind of detection method of residual amount of chloramphenicol
  • A kind of detection method of residual amount of chloramphenicol

Examples

Experimental program
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Embodiment 1

[0043] A kind of detection method of chloramphenicol residue, comprises the steps:

[0044] 1) Sample pretreatment: Take the aquatic product shrimp to be tested, take 5g of the muscle part and put it in a centrifuge tube, add 20mL of ethyl acetate, homogenize it with a homogenizer for 1min to make a homogenate, centrifuge at 4000r / min for 3min, and dissolve the ethyl acetate Transfer the ester layer to a thin-necked heart-shaped bottle; then add 10 mL of ethyl acetate to the centrifuge tube, homogenize for 1 min, centrifuge at 4000 r / min for 3 min, combine the ethyl acetate extract, and evaporate under reduced pressure in a water bath at 40 °C to dryness;

[0045] 2) Purification of the sample: Dissolve the extract obtained by evaporation in a water bath in step 1) in 1 mL of methanol, add 15 mL of n-hexane and 25 mL of 4% sodium chloride solution in turn, shake and mix for 1 min, then transfer to a centrifuge tube, 4000 r / min Centrifuge for 2 min, discard the upper n-hexane p...

Embodiment 2

[0051] A kind of detection method of chloramphenicol residue, comprises the steps:

[0052] 1) Sample pretreatment: Take the aquatic product shrimp to be tested, take 5g of the muscle part and put it in a centrifuge tube, add 20mL of ethyl acetate, homogenize it with a homogenizer for 1min to make a homogenate, centrifuge at 4000r / min for 3min, and dissolve the ethyl acetate Transfer the ester layer to a thin-necked heart-shaped bottle; then add 10 mL of ethyl acetate to the centrifuge tube, homogenize for 1 min, centrifuge at 4000 r / min for 3 min, combine the ethyl acetate extract, and evaporate under reduced pressure in a water bath at 40 °C to dryness;

[0053] 2) Purification of the sample: Dissolve the extract obtained by evaporation in a water bath in step 1) in 1 mL of methanol, add 15 mL of n-hexane and 25 mL of 4% sodium chloride solution in turn, shake and mix for 1 min, then transfer to a centrifuge tube, 4000 r / min Centrifuge for 2 min, discard the upper n-hexane p...

Embodiment 3

[0059] A kind of detection method of chloramphenicol residue, comprises the steps:

[0060] 1) Sample pretreatment: Take the aquatic product shrimp to be tested, take 5g of the muscle part and put it in a centrifuge tube, add 20mL of ethyl acetate, homogenize it with a homogenizer for 1min to make a homogenate, centrifuge at 4000r / min for 3min, and dissolve the ethyl acetate Transfer the ester layer to a thin-necked heart-shaped bottle; then add 10 mL of ethyl acetate to the centrifuge tube, homogenize for 1 min, centrifuge at 4000 r / min for 3 min, combine the ethyl acetate extract, and evaporate under reduced pressure in a water bath at 40 °C to dryness;

[0061]2) Purification of the sample: Dissolve the extract obtained by evaporation in a water bath in step 1) in 1 mL of methanol, add 15 mL of n-hexane and 25 mL of 4% sodium chloride solution in turn, shake and mix for 1 min, then transfer to a centrifuge tube, 4000 r / min Centrifuge for 2 min, discard the upper n-hexane ph...

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Abstract

The invention relates to a detection method for the residual quantity of chloramphenicol. The detection method includes the following steps of 1, sample pretreatment, wherein ethyl acetate is added into a sample, homogenizing and centrifugation are conducted, and then the mixture is evaporated to be almost dry; 2, purification of the sample, wherein normal hexane and an anhydrous sodium sulfate column are sequentially used for purifying the sample obtained in the step 1; 3, derivatization of the sample and a standard product, wherein acetic anhydride is adopted as a derivatization reagent, triethylamine is adopted as a catalyst, and the sample and the standard product are derived; 4, gas chromatography detection, wherein the sample solution and standard product solution obtained in the step 3 are injected into a gas chromatograph for detection. According to the detection method for the residual quantity of chloramphenicol, derivatization steps are simple, detection efficiency is high, the adopted derivatization reagent is low in sensitivity to the environment, the adopted catalyst is cheap, and harm to people and the environment is low.

Description

technical field [0001] The invention relates to the field of chloramphenicol detection, in particular to a method for detecting residual chloramphenicol in aquatic products. Background technique [0002] Chloramphenicol is widely used in the treatment of infectious diseases in animals and has been widely used in the aquaculture industry, but it also brings serious residual problems. Chloramphenicol can inhibit the hematopoietic function of human bone marrow and cause anemia, etc. . Therefore, the detection of chloramphenicol in aquatic products has special significance. [0003] Domestic and foreign literature reports that the detection methods of chloramphenicol drugs mainly use gas chromatography, gas chromatography-mass spectrometry (GC / MS) and liquid chromatography-mass spectrometry (LC / MS). Gas chromatography-mass spectrometry (GC / MS) and liquid chromatography-mass spectrometry (LC / MS) have high sensitivity, but are expensive. Generally, basic-level laboratories are n...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): G01N30/02G01N30/06G01N30/12
CPCG01N30/02G01N30/06G01N30/12G01N2030/025G01N2030/067G01N2030/126
Inventor 栾建文罗杰鸿吴济舟黄云生
Owner 国检测试控股集团京诚检测有限公司
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