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Preparing device and method for nanofiller capillary chromatography microcolumn

A technology for capillary chromatography and nano-filling, which is applied to a nano-filling capillary chromatographic micro-column preparation device and the field of preparation thereof, can solve the problems of long preparation period, expensive equipment required for preparation, complicated preparation process of nano-filling capillary chromatographic micro-column, and the like. Simple and efficient method

Active Publication Date: 2014-09-10
XIAMEN UNIV
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  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] The present invention aims to overcome the problems of complex preparation process of nano-filler capillary chromatography micro-column, long preparation period, expensive equipment required for preparation, etc., and provides one-time continuous filling of nano-filler by using the centrifugal force of the centrifuge instead of the high hydraulic pressure of the mechanical pump, and the operation is simple , a nano-filler capillary chromatography micro-column preparation device and its preparation method which is short in time and supports batch preparation

Method used

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  • Preparing device and method for nanofiller capillary chromatography microcolumn
  • Preparing device and method for nanofiller capillary chromatography microcolumn
  • Preparing device and method for nanofiller capillary chromatography microcolumn

Examples

Experimental program
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Effect test

Embodiment 1

[0034] Example 1: Alkyl modified SiO 2 Preparation of Nano-filled Capillary Chromatography Microcolumns

[0035] a Alkyl modified SiO 2 Synthesis of nanofillers

[0036] Mix absolute ethanol, water and ammonia water in a volume ratio of 47:9:14 into a round-bottomed flask, magnetically stir and mix evenly, and add the above 1 / 14 volume tetraethyl orthosilicate while stirring. Closed and stirred at a certain temperature for 6-10 hours; then add half volume of tetraethyl orthosilicate, absolute ethanol, water, etc. under stirring state, continue to react for 6-10 hours, age for 1-2 hours, centrifuge and wash for at least 3 times, washed with ethanol at least 3 times, dried at 110°C for 4-6 hours, and within 16 hours after cooling, the temperature was programmed from room temperature to 600-650°C in a muffle furnace. image 3 and 4 For the synthesized SiO 2 Scanning electron microscope (SEM) and transmission electron microscope (TEM) images of nano fillers show that the synt...

Embodiment 2

[0048] Example 2: SiO 2 Preparation of Au-S-C18 nano-packed column for capillary chromatography enrichment

[0049] a SiO 2 Preparation of Au-S-C18 Core-Shell Nanofillers

[0050] First, a certain amount of SiO prepared according to Example 1 2 Disperse the nanospheres in 10mL of 1:1 methanol and water solution, prepare 90mL of 0.03M SnCl 2 The solution was mixed with the above-mentioned nanoparticle dispersion, reacted for 45min under magnetic stirring, and dispersed in 4mL water after being washed by centrifugation for 8 times; secondly, 1.5mL1g / 100mL chloroauric acid was added to the 2 CO 3 100mL of water, react in dark for at least 24h to form aging solution. Add 1mL SiO to 50mL aging solution 2 sn 2+ For dispersion liquid, add hydroxylamine hydrochloride solution of appropriate concentration drop by drop under magnetic stirring until the reaction solution is bright blue, react for 8-10 hours, then age for 1 hour, wash with water at least 6 times, and then dry overn...

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Abstract

The invention discloses a preparing device and method for a nanofiller capillary chromatography microcolumn, and relates to preparation of nanofiller capillary chromatography microcolumns. The preparing device for the nanofiller capillary chromatography microcolumn is provided with a centrifugal machine and a centrifugal filling device. The centrifugal filling device is provided with a detachable PEEK joint, a PEEK interface, a PTFE sleeve, a capillary tube and a centrifugal tube. The method comprises the steps of taking nano particles to be dispersed into acetone, controlling the concentration to be 1 microgram / microliter to 50 micrograms / microliter, evenly mixing the homogenized solution, then conducting oscillation to obtain a homogenate, cutting out a segment of the elastic quartz capillary tube, pressing one single through hole silicon ball with the particle size slightly larger than the inner diameter of the capillary tube into one end of the capillary tube to be used as an outlet plunger, fixing the capillary tube with the outlet plunger into the centrifugal filling device, filling a liquid storage tank with the homogenate, conducting weighting and centrifuging, conducing fixed-phase filling, taking off the filled capillary tube after centrifuging is completed, filling the inlet end of the capillary tube with one through hole silica gel particle used as an inlet plunger, and obtaining the nanofiller capillary chromatography microcolumn.

Description

technical field [0001] The invention relates to the preparation of nano-filler capillary chromatographic micro-columns, in particular to a nano-filler capillary chromatographic micro-column preparation device and a preparation method for preparing nano-filler capillary chromatographic micro-columns simply, quickly and in batches. Background technique [0002] With the vigorous development of proteomics and metabolomics research, the current chromatographic separation technology is difficult to meet the requirements of high resolution, high selectivity and rapid analysis, so there is an urgent need for new high-efficiency and high-specificity chromatographic stationary phases. Due to their uniform particle size distribution, high specific surface area, rich surface modification chemistry and excellent stability, nanomaterials have gradually attracted people's attention to their chromatography applications. Studies have shown that whether used as chromatographic fillers or enr...

Claims

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Application Information

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IPC IPC(8): G01N30/60
Inventor 张博王林周拙恒刘娅
Owner XIAMEN UNIV
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