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Ionic liquid bridged hybrid silicon oxide serving as water-rich chromatographic stationary phase as well as preparation method and application of ionic liquid bridged hybrid silicon oxide

A chromatographic stationary phase, water-enriched technology, applied in chemical instruments and methods, alkali metal oxides/hydroxides, inorganic chemistry, etc., can solve the change of analyte retention characteristics, decrease of chromatographic column selectivity, decrease of column efficiency, etc. question

Active Publication Date: 2020-10-30
镇江海关综合技术中心
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  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005]In the PALC mode, a high proportion of water needs to be used as the mobile phase, which is a great test for the service life of the separation material, and the following problems need to be solved : (1) General stationary phases, such as C18, after using rich water mobile phases for a long time, the column efficiency will be seriously reduced, especially when there are silanols exposed
(2) The pH range that can be used is narrow; when pH>8, silica gel is easy to dissolve; when pH<2, the bonded silica gel stationary phase will be lost, so that the retention characteristics and peak shape of the analyte change, and the selectivity of the chromatographic column reduce
(3) When analyzing alkaline substances, the exposed silanic hydroxyl groups on the surface of silica gel have an irreversible adsorption effect on alkaline substances, especially N-containing compounds, and easily denature biological macromolecules, especially polypeptides, proteins, etc., resulting in non-specific adsorption. , resulting in severe tailing of chromatographic peaks and lower recovery

Method used

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  • Ionic liquid bridged hybrid silicon oxide serving as water-rich chromatographic stationary phase as well as preparation method and application of ionic liquid bridged hybrid silicon oxide
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  • Ionic liquid bridged hybrid silicon oxide serving as water-rich chromatographic stationary phase as well as preparation method and application of ionic liquid bridged hybrid silicon oxide

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Experimental program
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Embodiment 1

[0116] Example 1. Preparation of Ionic Liquid Bridged Hybrid Silica as Stationary Phase for Water-rich Chromatography

[0117] Experimental principle

[0118] This reaction system is mainly composed of silicon source, template molecule, cosolvent, catalyst (acid or base) and pore expander. With BTMSPICl and BTSE as di-silicon sources, cationic surfactant octadecyltrimethylammonium chloride (Octadecyltrimethylammonium chloride, C 18 TACl) as a template, ethanol and water as a mixed co-solvent, and N,N-dimethyldecylamine (DMDA) as a pore-enlarging agent, under alkaline conditions and nitrogen protection, through one-step co-condensation Spherical ILs bridged mesoporous organosilica (PMO-ILs), the synthesis diagram is shown in figure 1 .

[0119] Experimental part

[0120] Experimental Materials and Instruments

[0121] Main materials and reagents

[0122] Sodium imidazole, (3-chloropropyl)trimethoxysilane, 1,2-bis(triethoxysilyl)ethane (1,2-Bis(triethoxysilyl)ethane, BTSE)...

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Abstract

The invention discloses ionic liquid bridged hybrid silicon oxide serving as a water-rich chromatographic stationary phase as well as a preparation method and application of the ionic liquid bridged hybrid silicon oxide. The invention provides a novel hydrophilic stationary phase PMO-ILs-Au NPs which is environmentally friendly. The novel stationary phase has the characteristics of HILIC and PALC,and same as the HILIC, the PALC can retain polar compounds. The stationary phase can separate organic acids, biogenic amines and other polar compounds, and has the advantages of high separation degree and favorable selectivity. The invention also establishes a PALC-MS / MS detection method of eight biogenic amine compounds in aquatic products, the operation is simple, accurate and rapid, the separation effect is good, synchronous analysis of the eight biogenic amine compounds can be realized, and the detection requirements of common biogenic amine compounds in food can be met.

Description

technical field [0001] The invention belongs to the field of food testing, and relates to an ionic liquid bridging hybrid silicon oxide used as a stationary phase of water-rich chromatography, a preparation method and application thereof. Background technique [0002] Food additives are widely used in food production and are an important part of the modern food industry. According to national regulations, there are only more than 2,000 food additives allowed to be used in food, and some unscrupulous manufacturers lack integrity and add some illegal ingredients to processed foods to increase the color and taste of food or counterfeit main ingredients. The proliferation of illegal additives has brought great harm to my country's food safety. In recent years, food safety issues have been exposed frequently, such as dicyandiamide and melamine incidents in dairy products, "leather milk" incidents, malachite green incidents in aquatic products, clenbuterol in feed, sodium copper ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J20/285B01J20/28G01N30/02
CPCB01J20/285B01J20/28011B01J20/28061B01J20/28064B01J20/28083B01J20/28073B01J20/28076B01J20/28021G01N30/02
Inventor 陈桐宋广三肖震李炳祥徐亮徐虹沈伟健杨敏吴艳玲
Owner 镇江海关综合技术中心
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