Method for detecting sulfadimidine in veterinary Shuanghuanglian oral liquid

A technology of Shuanghuanglian oral liquid and sulfamethazine, which is applied in measurement devices, instruments, scientific instruments, etc., can solve the problems of sample turbidity, inaccurate sample detection results, and high detection limit of detection methods, and achieves strong repeatability. , the effect of low detection limit

Active Publication Date: 2020-12-18
北京精益捷检测科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Although there are various national standards in the field of food safety testing to detect and supervise the residues of sulfamethazine in food (i.e. meat products made from livestock and poultry), there is no source for the residues of sulfa drugs ( (i.e. veterinary drugs eaten by livestock, poultry, etc.) testing methods or the issuance of relevant testing standards
[0005] When using relevant national standards or detection methods for the detection of sulfamethazine in the veterinary drug Shuanghuanglian oral liquid, when the sample of the veterinary drug Shuanghuanglian oral liquid to be tested is pretreated, the sample obtained after the pretreatment often appears turbid, As a result, the detection results of the samples are inaccurate, and the detection limit of the detection method is too high

Method used

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  • Method for detecting sulfadimidine in veterinary Shuanghuanglian oral liquid
  • Method for detecting sulfadimidine in veterinary Shuanghuanglian oral liquid
  • Method for detecting sulfadimidine in veterinary Shuanghuanglian oral liquid

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Embodiment 1

[0047] A method for detecting sulfamethazine in the veterinary drug Shuanghuanglian oral liquid, comprising the following steps: S1. Take 1 g (accurate to 0.01g) of the veterinary drug Shuanghuanglian oral liquid to be detected in a 50mL centrifuge tube, add 4mL deionized water to dissolve Afterwards, mix well, add 20mL acetonitrile to extract again, obtain extract; Wherein, acetonitrile is used as extract, and the total volume of extract is recorded as V 1 , mL.

[0048] S2. Add 3g of sodium chloride to the extract, mix well, and vibrate the centrifuge tube containing the liquid (including veterinary drug Shuanghuanglian oral liquid and deionized water) for 10 minutes with a speed-regulating multi-purpose oscillator, then use a laboratory centrifuge Centrifuge at 4000r / min for 5min to obtain supernatant 1.

[0049] S3. Take 10 mL of the supernatant 1 and dry it under a nitrogen blower at 50°C to remove the acetonitrile in the supernatant 1 to obtain a residue; wherein, the v...

Embodiment 2

[0053] The difference between this embodiment and Embodiment 1 is that the setting parameters of each operation in this embodiment are different, specifically including the following steps:

[0054] S1. Take 1 g (accurate to 0.01 g) of the veterinary drug Shuanghuanglian oral liquid to be tested in a 50 mL centrifuge tube, add 8.3 mL of deionized water to dissolve, mix well, and then add 25 mL of acetonitrile for extraction to obtain an extract.

[0055] S2. Add 3.32g of sodium chloride to the extract, mix well and oscillate for 13min with a vortex shaker at a speed of 1000r / min, then use a laboratory centrifuge to centrifuge at a speed of 3000r / min for 8min to obtain a supernatant 1.

[0056] S3. Take 10 mL of the supernatant and dry it under a nitrogen blower at 50° C. to remove the acetonitrile in the supernatant 1 to obtain a residue.

[0057] S4. After adding 1 mL of a 0.01 mol / L phosphate buffer-methanol mixed solution with a pH of 7.0 to the residue, vortex and mix to ...

Embodiment 3

[0061] The difference between this embodiment and Embodiment 1 is that the setting parameters of each operation in this embodiment are different, specifically including the following steps:

[0062] S1. Take 1 g (accurate to 0.01 g) of the veterinary drug Shuanghuanglian oral liquid to be tested in a 50 mL centrifuge tube, add 1 mL of deionized water to dissolve, mix well, add 8 mL of acetonitrile for extraction, and obtain an extract.

[0063] S2. Add 3g of sodium chloride to the extract, mix well and oscillate for 12min with a vortex shaker at a speed of 5000r / min, then centrifuge for 5min at a speed of 5000r / min in a laboratory centrifuge to obtain supernatant 1 .

[0064] S3. Take 6.7 mL of the supernatant and dry it under a nitrogen blower at 50° C. to remove the acetonitrile in the supernatant 1 to obtain a residue.

[0065] S4. After adding 1 mL of a 0.01 mol / L phosphate buffer-methanol mixed solution with a pH of 7.0 to the residue, vortex and mix to obtain a reconsti...

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Abstract

The invention discloses a method for detecting sulfadimidine in veterinary Shuanghuanglian oral liquid, belongs to the technical field of detection methods, and solves the problems of inaccurate detection result of a sample and overhigh detection limit of a detection method due to turbidity of the sample in an existing detection method. The detection method comprises the following steps: S1, adding deionized water and acetonitrile into a to-be-detected sample to obtain an extracting solution; S2, adding sodium chloride into the extracting solution, uniformly mixing, oscillating, and centrifuging to obtain a supernatant 1; S3, subjecting the supernatant 1 to nitrogen blowing to obtain residue; S4, adding a mixed solution of a phosphate buffer solution and methanol into the residues, and uniformly mixing the liquid to obtain a redissolved solution; and S5, centrifuging the redissolved solution, filtering the liquid through a micro-filtration membrane to obtain a supernatant 2, filteringthe supernatant 2, and carrying out liquid chromatography tandem mass spectrometer detection. The detection method has the advantages of being low in detection limit and accurate in detection.

Description

technical field [0001] The application relates to the technical field of drug detection, more specifically, it relates to a method for detecting sulfamethazine in veterinary medicine Shuanghuanglian oral liquid. Background technique [0002] Sulfonamides are artificially synthesized antibacterial drugs, which have the advantages of broad antibacterial spectrum, stable properties, and easy use. However, sulfonamides are prone to drug resistance, and the metabolites in the liver are acetylated sulfonamides. The solubility of acetylated sulfonamides is low, and they are easy to precipitate and crystallize in urine, causing damage to the kidneys. Therefore, sulfonamides in the human body must be strictly controlled. drug intake. In addition to active drug use, ingestion through food is also a way for sulfa drugs to enter the human body, so it is necessary to strictly control the content of sulfa drugs in food intake. One of the ways for sulfa drugs to enter the human body thro...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N30/02G01N30/06G01N30/34G01N30/72G01N30/86
CPCG01N30/02G01N30/06G01N30/34G01N30/72G01N30/8675G01N2030/062
Inventor 张萌萌李宗进姬桂花郭超晖李震杜志毅王璐
Owner 北京精益捷检测科技有限公司
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