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A monolithic column and graphene technology, applied in the field of analytical chemistry, can solve the problems of cumbersome offline steps, time-consuming and laborious, etc., and achieve high-efficiency and rapid extraction effects, wide application range, and high enrichment multiples
Active Publication Date: 2019-05-31
INSPECTION & QUARANTINE TESTING CENT OF HEBEI ENTRY EXIT INSPECTION & QUARANTINE BUREAU
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However, the offline method is cumbersome, time-consuming and laborious. The online solid-phase extraction method automates the offline solid-phase extraction process, reduces the degree of human participation, improves the reproducibility of the analytical method, and overcomes the shortcomings of the offline solid-phase extraction method. Therefore, the online The application of solid phase extraction instruments is also becoming more and more popular
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Embodiment 1
[0023] Embodiment 1: the preparation method of ploy (GO-co-EDMA) monolithic column
[0024] Take 1.7 mg of GO in a centrifuge tube, add 1850 μL of porogen, 650 μL of cross-linking agent EDMA, 1.0 mg of azobisisobutyronitrile (AIBN), ultrasonically mix and degas. Pour the uniformly mixed liquid into a stainless steel tube (10mm×2.1mm) with one end sealed, and seal the other end. React in a water bath at 60°C for 30 hours to obtain a poly(GO-co-EDMA) monolithic column. After the reaction is completed, it is connected to a high-performance liquid chromatography system, and the monolithic column is washed with methanol to remove unreacted monomers and porogens to obtain an online purified monolithic column. The scanning electron microscope picture of the monolithic column section of the obtained product is as follows figure 1 shown.
Embodiment 2
[0025] Embodiment 2: the preparation method of ploy (GO-co-EDMA) monolithic column
[0026] Take 1.5 mg of GO in a centrifuge tube, add 1550 μL of porogen, 650 μL of cross-linking agent EDMA, 1.0 mg of azobisisobutyronitrile (AIBN), ultrasonically mix and degas. Pour the uniformly mixed liquid into a stainless steel tube (10mm×2.1mm) with one end sealed, and seal the other end. React in a water bath at 65°C for 30 hours to obtain a Poly(GO-co-EDMA) monolithic column. After the reaction is completed, it is connected to a high-performance liquid chromatography system, and the monolithic column is washed with methanol to remove unreacted monomers and porogens to obtain an online purified monolithic column. The scanning electron microscope picture of the monolithic column section of the obtained product is as follows figure 2 shown
Embodiment 3
[0027] Example 3: Using the monolithic column prepared in Example 1 as the extraction medium, combined with liquid chromatography tandem mass spectrometry, on-line purification analysis and detection of sulfa drugs in chicken
[0028] (1) extraction
[0029] Weigh about 2g of ground chicken sample, add 2g of anhydrous sodium sulfate and 20mL of acetonitrile, extract homogeneously for 1min, centrifuge at 4000rpm for 10min, take 5mL of the supernatant and blow it to dryness with nitrogen at 40°C, and dissolve it in 1mL of 5mmol / L ammonium acetate aqueous solution The residue was passed through a 0.45 filter membrane for back-up online purification liquid chromatography tandem mass spectrometry analysis.
[0030] (2) Online purification
[0031] The online SPE conditions are divided into 4 parts: loading, washing, elution and conditioning. The sample passes through a poly(GO-co-EDMA) online solid-phase extraction column, and the target analytes are retained on the purification ...
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Abstract
The invention belongs to the field of analytic chemistry and particularly relates to a graphene oxide type online purification and solid-phase extraction monolithic column and a preparation method and application thereof. The graphene oxide type online purification and solid-phase extraction monolithic column comprises a stainless steel tube, and a monolithic column body generated by in-situ polymerization is arranged in the stainless steel tube and refers to a polymer of graphene oxide and ethylene glycol dimethacrylate. The preparation method includes subjecting a GO (graphite oxide) monomer, a mixed porogenic agent, a cross-linking agent and an initiator to ultrasonic mixing and degasification; sealing the mixture in the stainless steel tube for water bath polymerization reaction and flushing the mixed porogenic agent and unreacted monomers away by methyl alcohol. The graphene oxide type online purification and solid-phase extraction monolithic column has the advantages that through a mode of the monolithic column, the advantages of large specific surface area, high property stability and the like of a graphene oxide material are given to full lay, and the graphite oxide is doped into the polymer to form the graphene oxide-polymer monolithic column; the monolithic columns serve as online purification columns, so that a novel method for analyzing veterinary drug residues in animal-derived food simply and quickly is established.
Description
technical field [0001] The invention belongs to the field of analytical chemistry, and in particular relates to a graphene oxide-type on-line purification solid-phase extraction monolithic column, a preparation method and an application. Background technique [0002] In recent years, food safety incidents have occurred frequently, and people's awareness of food safety has become higher and higher. This has made both government regulatory agencies, food production and sales companies strengthen food safety risk control, and the testing work of food testing laboratories has become more and more serious. onerous. As an important purification means of pretreatment - solid phase extraction method is also more and more widely used. However, the offline method is cumbersome, time-consuming and laborious. The online solid-phase extraction method automates the offline solid-phase extraction process, reduces the degree of human participation, improves the reproducibility of the analy...
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Application Information
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Patent Type & Authority Patents(China)
IPC IPC(8): B01J20/285B01J20/30B01D15/08
CPCB01D15/08B01J20/285B01J2220/54
Inventor 艾连峰王曼曼马育松张海超
Owner INSPECTION & QUARANTINE TESTING CENT OF HEBEI ENTRY EXIT INSPECTION & QUARANTINE BUREAU
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