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Double-template molecularly-imprinted solid-phase extraction column and application method

A solid-phase extraction column, molecular imprinting technology, applied in separation methods, chemical instruments and methods, ion exchange, etc., can solve the problems of destroying the balance of normal flora in the human body, affecting the detection results, and affecting the accuracy of quantitative results.

Active Publication Date: 2016-01-13
JIANGSU UNIV
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  • Abstract
  • Description
  • Claims
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AI Technical Summary

Problems solved by technology

[0002] β-lactam antibiotics are a class of antibiotics widely used in the world. They are often used in the dairy industry because of their remarkable efficacy in treating bovine mastitis; It can lead to its residues in milk, frequent drinking of this kind of milk may cause allergic reactions in people with allergies, and may also destroy the balance of normal flora in the human body, leading to the emergence of drug-resistant bacteria; when detecting β-lactam antibiotic residues , low residues often require proper enrichment before detection; in addition, in multi-residue chromatographic detection, a large number of coexisting substrates in the sample are particularly likely to contaminate the chromatographic column, and purification is required to remove the substrate, even if no column contamination is used. For the problematic capillary electrophoresis method, due to the complex matrix of the sample, the signal of the matrix and the signal of the analyte may overlap, which affects the accuracy of the quantitative result. The sample also needs to be purified. For detection, enrichment and purification are very necessary
[0003] Solid-phase extraction has been widely used in sample pretreatment for veterinary drug residue detection, and has become one of the most common methods for enrichment and purification. However, the fillers used in solid-phase extraction columns are usually non-specific and selective adsorption materials. , in practical applications, the interfering substances are often extracted into the sample at the same time, which affects the detection results; moreover, commercial solid-phase extraction columns are mostly used for one-time use, which increases the detection cost; molecularly imprinted polymers are tailor-made for the template molecular weight Molecular polymers have high recognition for template molecules and their structural analogs, and can be reused many times, which are unmatched by ordinary solid phase extraction packing materials; currently reported molecularly imprinted solid phase extraction packing materials mostly use a single template Molecular synthesis, when used for sample pretreatment of similar veterinary drugs with many residues, such as β-lactams, some drugs in this type of veterinary drugs cannot be efficiently recognized by this single-template molecularly imprinted solid-phase extraction filler, resulting in The number of varieties of this type of veterinary drug that can be extracted in a sample pretreatment process is limited, which reduces the efficiency of enrichment and purification treatment of multiple residues of this type of veterinary drug

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  • Double-template molecularly-imprinted solid-phase extraction column and application method

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Embodiment 1

[0030] Preparation of oxacillin and cephalexin double-template molecularly imprinted solid-phase extraction column

[0031] A Mix and dissolve oxacillin (41.9mg), cephalexin (34.7mg) and acrylamide in 100mL methanol at a molar ratio of 1:1:8, vibrate ultrasonically for 10min, and place it overnight at room temperature. The molar ratio of cillin and cephalexin to ethylene glycol dimethacrylate is 1:1:40 and the molar ratio to azobisisobutyronitrile is 1:1:0.91, and the two are added to the above solution for ultrasonication Vibrate for 10 minutes, pass nitrogen gas into the container containing the solution for 5 minutes, seal the container, and then place it at 60 ° C reacted in a constant temperature water bath for 24 hours to prepare polymer microspheres, put the polymer microspheres in a Soxhlet extractor, wash off the template molecules with a mixed solvent of methanol-acetic acid with a volume ratio of 9:1, and then put them into vacuum drying Dry to constant weight.

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Embodiment 2

[0046] Preparation of oxacillin and cephalexin double-template molecularly imprinted solid-phase extraction column

[0047] A Mix oxacillin (40.7 mg), cephalexin (35.8 mg) and acrylamide in a molar ratio of 0.97:1.03:8 and dissolve in 100 mL of methanol, ultrasonically vibrate for 10 min, and place overnight at room temperature. The molar ratio of cillin and cephalexin to ethylene glycol dimethacrylate is 0.97:1.03:40 and the molar ratio to azobisisobutyronitrile is 0.97:1.03:0.91. Add the two to the above solution and ultrasonically Vibrate for 10 minutes, pass nitrogen gas into the container containing the solution for 5 minutes, seal the container, and then place it at 60 ° C reacted in a constant temperature water bath for 24 hours to prepare polymer microspheres, put the polymer microspheres in a Soxhlet extractor, wash off the template molecules with a mixed solvent of methanol-acetic acid with a volume ratio of 9:1, and then put them into vacuum drying Dry to constant ...

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Abstract

The invention relates to the technical field of solid-phase extraction, specifically to an oxacillin-and-cephalexin double-template molecularly-imprinted solid-phase extraction column and an application method. The extraction column is cooperatively used with a capillary electrophoresis method for selective separation, enrichment and detection of residues of amoxicillin, cephalexin, oxacillin, penicillin G, cefazolin sodium and cefoperazone sodium in animal food.

Description

technical field [0001] The invention relates to the technical field of solid-phase extraction, in particular to an oxacillin and cephalexin double-template molecularly imprinted solid-phase extraction column and its use method, which are combined with capillary electrophoresis for selective separation, enrichment and detection of animal food Residues of amoxicillin, cephalexin, oxacillin, penicillin G, cefazolin sodium and cefoperazone sodium. Background technique [0002] β-lactam antibiotics are a class of antibiotics widely used in the world. They are often used in the dairy industry because of their remarkable efficacy in treating bovine mastitis; It can lead to its residues in milk, frequent drinking of this kind of milk may cause allergic reactions in people with allergies, and may also destroy the balance of normal flora in the human body, leading to the emergence of drug-resistant bacteria; when detecting β-lactam antibiotic residues , low residues often require pro...

Claims

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Application Information

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IPC IPC(8): B01J20/285B01J20/30B01D15/08B01D15/22C08F220/56C08F222/14G01N1/34G01N27/26
Inventor 陈冠华郭利辉田一方梅晓芸洪月琴
Owner JIANGSU UNIV
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