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Solid-phase extraction method for various glucocorticoids and derivatives thereof in domestic drinking water

A technology for glucocorticoid and drinking water, which is applied in the directions of water pollutants, separation methods, chemical instruments and methods, etc., can solve the problems of limited specific surface area and functional group content, easy blockage of adsorbent pores, and high price. Achieve excellent stability, simple operation and cost saving effect

Pending Publication Date: 2021-09-07
大连海关技术中心
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0006] The present invention aims at the disadvantages of current traditional solid phase extraction materials such as limited specific surface area and functional group content, low recovery rate, easy blockage of adsorbent pores, high price, etc., and provides a kind of glucocorticoid and its derivatives in drinking water solid phase extraction method

Method used

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  • Solid-phase extraction method for various glucocorticoids and derivatives thereof in domestic drinking water
  • Solid-phase extraction method for various glucocorticoids and derivatives thereof in domestic drinking water
  • Solid-phase extraction method for various glucocorticoids and derivatives thereof in domestic drinking water

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Experimental program
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Effect test

Embodiment 1

[0032] Cleaning of the column tube of the solid phase extraction column: select a 3ml solid phase extraction column (length: 6.3cm inner diameter: 8.9mm diameter: 9.0mm), check whether the appearance is intact and not damaged, clean with methanol and acetone in sequence, and remove the grease on the surface of the column tube , and then rinsed with tap water, and finally rinsed with distilled water and acetone, and dried thoroughly under natural conditions for later use.

[0033] Preparation of toluene-triphenylbenzene porous organic framework material: 1,3,5-triphenylbenzene and toluene were used as materials through Friedel-Craft alkylation reaction, with ferric chloride as catalyst and dichloroethane as The solvent is heated to 80° C. under vigorous stirring to uniformly polymerize 1,3,5-triphenylbenzene and toluene to obtain a toluene-triphenylbenzene porous organic framework material.

[0034] Solid-phase extraction column preparation: select 3ml solid-phase extraction co...

Embodiment 2

[0038] According to the preparation method of the solid phase extraction column, the solid phase extraction column tube of the same specification is adopted to prepare the solid phase extraction column with the filling amount of 10mg, 15mg, 20mg, and 25mg respectively. Taking blank distilled water as the sample, 13 kinds of glucocorticoids and Its derivatives (cortisone, hydrocortisone, hydrocortisone butyrate, dexamethasone, methylprednisolone, betamethasone acetate, fluorometholone, flumethasone, beclomethasone, prednisone , triamcinolone acetonide, budesonide, fludrocetone) for addition and recovery experiments, the addition level was 1.0 μg / L, according to the water sample solid phase extraction procedure, the water sample was enriched and concentrated, and the high performance liquid chromatography-four Pole / electrostatic field orbitrap high-resolution mass spectrometry (UPLC-Q-Exactive MS) for analysis and testing, chromatographic conditions: Chromatographic column: Therm...

Embodiment 3

[0042] Taking blank distilled water as a sample, select 22 kinds of glucocorticoids and their derivatives (prednisone, cortisone, triamcinolone diacetate, hydrocortisone, flumethasone, dexamethasone, fludrocortisone acetate) , prednisone acetate, beclomethasone, methylprednisolone, cortisone acetate, hydrocortisone acetate, betamethasone acetate, fluorometholone, fludrosulfone, deflazacort, triamcinolone acetonide , methylprednisolone acetate, hydrocortisone butyrate, budesonide), the addition and recovery experiments of different concentration levels were carried out, the addition levels were 0.4, 1.0, 2.0μg / L, and the filler amount was 20mg respectively The solid phase extraction column enriches and concentrates the water sample, adopts high-performance liquid chromatography-quadrupole / electrostatic field orbitrap high-resolution mass spectrometry (UPLC-Q-Exactive MS) to carry out analysis test, and chromatographic conditions and mass spectrometry conditions are the same as e...

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Abstract

The invention relates to a solid-phase extraction technology, in particular to a solid-phase extraction method for various glucocorticoids and derivatives thereof in domestic drinking water. According to the solid-phase extraction method, a methylbenzene-sym-triphenylbenzene porous organic framework material is used as a filler, a small solid-phase extraction column is manufactured, and the glucocorticoid and the derivative of the glucocorticoid in the domestic drinking water are obtained. The methylbenzene-sym-triphenylbenzene solid-phase extraction column prepared by the invention has higher stability, and can enrich various glucocorticoids and derivatives thereof in domestic drinking water; and the prepared methylbenzene-sym-triphenylbenzene solid-phase extraction column is simple to operate when being used, and can be repeatedly used, so that the cost is saved, and the environmental pollution is avoided.

Description

technical field [0001] The invention relates to solid-phase extraction technology, in particular to a solid-phase extraction method for various glucocorticoids and derivatives thereof in drinking water. Background technique [0002] As pharmaceuticals, glucocorticoids are widely used in human and animal medicine. They can regulate the synthesis and metabolism of sugar, fat and protein, and are mainly used for the treatment of diseases such as anti-inflammatory response and immunosuppression. Glucocorticoids have strong polarity and are not easily adsorbed on organisms, so that 50%-60% of glucocorticoids are quickly excreted with urine and feces, and enter the environment through various channels. Drug use, domestic sewage, medical wastewater, and wastewater from agriculture, animal husbandry, fishery and aquaculture are the main sources of glucocorticoids in environmental water. Drugs ingested by humans or animals enter the environment in the form of original drugs or their...

Claims

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Application Information

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IPC IPC(8): C02F9/02B01J20/22B01D15/20B01D15/12G01N30/02G01N30/06G01N30/72G01N30/86C02F101/34C02F101/38
CPCC02F1/44C02F1/26B01J20/226B01D15/206B01D15/125G01N30/02G01N30/06G01N30/7266G01N30/8675G01N2030/047G01N2030/062C02F2101/34C02F2101/38
Inventor 褚莹倩吴慈陈溪张晓林
Owner 大连海关技术中心
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