Purifying filler for sulfonamide residues and pretreatment method

A purification column and alumina technology, applied in chemical instruments and methods, separation methods, other chemical processes, etc., can solve the problems of complex operation, high proportion of organic solvents used, high matrix effect, etc., and achieve wide applicable matrix and good stability , High recovery effect

Pending Publication Date: 2022-06-28
SHENZHEN BIOEASY BIOTECHNOLOGY CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] At present, the pretreatment method in the prior art has the following disadvantages: (1) The traditional liquid-liquid extraction has limited effect on removing impurities, which leads to a high matrix effect of subsequent liquid chromatography-tandem mass spectrometry, which interferes with the accuracy of the results to a certain extent, and at the same time Causes a certain degree of damage to the instrument; (2) Liquid-liquid extraction requires multi-step extraction, the use of organic solvents is high, has certain toxicity, and requires rotary evaporation, and the steps are complicated; (3) Solid-phase extraction requires activation, sample loading, Steps such as rinsing and elution are complicated to operate; (4) dispersive solid-phase extraction requires an additional step-centrifugation, and there is no theoretical plate effect, and the adsorption of impurities is limited

Method used

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  • Purifying filler for sulfonamide residues and pretreatment method
  • Purifying filler for sulfonamide residues and pretreatment method
  • Purifying filler for sulfonamide residues and pretreatment method

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0068] Example 1. Verification of the detection effect of sulfonamide drug residues in pork samples

[0069] In Example 1, pork with different concentrations of standard products was used as a sample, and 0.5 g of salt package (sodium sulfate: sodium chloride (mass ratio) = 1:1) and silica gel, alumina and HLB (mass ratio) were used. A solid-phase purification column composed of 1:2:0.5 and a total filler content of 2g). The purified sample extract was diluted 10 times with the initial mobile phase, filtered through a 0.22 μm filter membrane, and finally analyzed by UPLC-MS / MS.

[0070] Test results: under different standard concentrations, the average recoveries obtained were between 70% and 108%, and the RSDs were all less than 15% (see Table 3). It can be seen that this pretreatment method is a qualified sulfonamide drug pretreatment method.

[0071] Table 3. Recovery accuracy and precision of sulfonamide residues in pork samples

[0072]

[0073]

[0074]

Embodiment 2

[0075] Example 2. Verification of the detection effect of sulfonamide drug residues in beef samples

[0076] In Example 2, beef with different concentrations of standard substances was used as the sample, and 1 g of salt package (sodium sulfate: sodium chloride (mass ratio) = 1:0.5) and silica gel, alumina and HLB (mass ratio of 1:3:1, a solid-phase purification column composed of a total filler content of 2g). Take 500 μL of the purified sample extract and blow it dry with nitrogen, reconstitute it with 1 mL of the initial mobile phase, filter it through a 0.22 μm filter membrane, and finally conduct UPLC-MS / MS analysis.

[0077] Test results: under different standard concentrations, the average recovery rate obtained is between 73% and 102%, and the RSD is less than 15% (see Table 4), which is within the scope of the national standard for sulfonamides. It can be seen that this pretreatment method is a qualified sulfonamide drug pretreatment method.

[0078] Table 4. Recove...

Embodiment 3

[0082] Example 3. Verification of the detection effect of sulfonamide drug residues in chicken samples

[0083] In Example 2, chickens with different concentrations of standard products were used as samples, and 0.2 g of salt package (sodium sulfate: sodium chloride (mass ratio) = 1:1) and silica gel, alumina and HLB (mass ratio of 1:0.5:0.5, the total content of filler is 1.5g) of solid phase purification column. Take 200 μL of the purified sample extract and blow dry with nitrogen, reconstitute it with 1 mL of the initial mobile phase, filter it through a 0.22 μm filter membrane, and finally conduct UPLC-MS / MS analysis.

[0084] Test results: under different standard concentrations, the average recovery rate obtained is between 81% and 113%, and the RSD is less than 15% (see Table 5), which is within the scope of the national standard for sulfonamides. It can be seen that this pretreatment method is a qualified sulfonamide drug pretreatment method.

[0085] Table 5. Recove...

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Abstract

The invention relates to the field of drug residue detection, in particular to a purification filler for sulfonamide drug residues, a solid-phase purification column containing the filler and a corresponding pretreatment method. According to the solid-phase purification column and the pretreatment method, the adsorption principle of the mixed filler is utilized, various impurities in the to-be-detected sample can be simply and quickly removed, the operation is simple and convenient, and a detection result with good stability and high recovery rate is ensured to be obtained under the condition that calibration of a matrix standard curve is not needed.

Description

technical field [0001] The invention relates to the field of drug residue detection, and more particularly, to a purification filler and a corresponding pretreatment method. Background technique [0002] Sulfonamides (SAs) are a class of synthetic antibiotics with a p-aminobenzenesulfonamide structure, which can inhibit the growth and reproduction of bacteria and have strong antibacterial effects. It has excellent characteristics such as low cost and convenient use, and is widely used in the prevention and treatment of animal husbandry diseases. However, the abuse, misuse and non-compliance with the withdrawal period of sulfonamide drugs will result in excessive sulfonamide residues in animal-derived foods, and sulfonamide drugs are not easily metabolized, so they will accumulate in the human body and cause various potential hazards to the human body. In addition, sulfonamides also have serious side effects and potential carcinogenicity, and the problem of drug resistance i...

Claims

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Application Information

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IPC IPC(8): B01J20/26B01J20/30B01D15/10B01D15/22B01D36/00G01N1/34
CPCB01J20/103B01J20/08B01J20/26B01D15/10B01D36/00G01N1/34B01J2220/4812B01J2220/4806B01J2220/46
Inventor 何洁严义勇梁松余婷婷
Owner SHENZHEN BIOEASY BIOTECHNOLOGY CO LTD
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