A nano-filler capillary chromatography micro-column preparation device and preparation method thereof

A technology of capillary chromatography and nanofiller, which is applied in the field of nanofiller capillary chromatography microcolumn preparation device and its preparation, can solve the problems of long preparation cycle, complicated preparation process of nanofiller capillary chromatography microcolumn, expensive equipment required for preparation, etc., to achieve The method is simple and efficient

Active Publication Date: 2016-07-27
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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  • A nano-filler capillary chromatography micro-column preparation device and preparation method thereof
  • A nano-filler capillary chromatography micro-column preparation device and preparation method thereof
  • A nano-filler capillary chromatography micro-column preparation device and preparation method thereof

Examples

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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] aSiO 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 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 overnight at 50-...

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Abstract

The invention discloses a nano-filler capillary chromatographic micro-column preparation device and a preparation method thereof, which relate to the preparation of a nano-filler capillary chromatographic micro-column. The nano-filler capillary chromatography microcolumn preparation device is provided with a centrifuge and a centrifugal filling device, and the centrifugal filling device is provided with a detachable PEEK joint, a PEEK interface, a PTFE sleeve, a capillary and a centrifuge tube. Take nanoparticles and disperse them in acetone, the concentration is controlled at 1-50 μg / μL, and the homogenate solution is mixed and oscillated to obtain a homogenate solution; a section of elastic quartz capillary is cut off, and a single through-hole silicon ball with a particle size slightly larger than the inner diameter of the capillary is pressed into the capillary One end is used as the outlet plunger; fix the capillary with the outlet plunger in the centrifugal filling device, inject the homogenate into the liquid storage tank, weigh and centrifuge, and fill the stationary phase; after the centrifugation is completed, remove the filled capillary, A through-hole silica gel particle is filled at the inlet end of the capillary as an inlet plunger to obtain a nano-filled capillary chromatographic 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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Patent Type & Authority Patents(China)
IPC IPC(8): G01N30/60
Inventor 张博王林周拙恒刘娅
Owner XIAMEN UNIV
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