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Mixed capillary chromatographic column with shower head and preparation method thereof

A capillary chromatographic column, mixed-type technology, applied in the field of preparation of mixed-type capillary chromatographic columns, can solve problems affecting the performance of capillary tubes, scrapping of capillary chromatographic columns, clogging of chromatographic fillers, etc., achieve low cost, shorten service life, and high-efficiency separation The effect of the analysis

Inactive Publication Date: 2010-12-22
INST OF RADIATION MEDICINE ACAD OF MILITARY MEDICAL SCI OF THE PLA
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] At present, the main problem with capillary columns used in LC-MS is that although capillary columns with tapered nozzles can significantly improve the sensitivity compared with the previous direct use of hollow capillary nozzles, the nozzle end of such columns is generally Without a sieve plate, as the pressure of the packing on the nozzle increases gradually and the use time prolongs, the gap near the nozzle will be blocked by broken chromatographic packing, which will affect the performance of the capillary and even make the capillary column scrapped

Method used

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  • Mixed capillary chromatographic column with shower head and preparation method thereof
  • Mixed capillary chromatographic column with shower head and preparation method thereof
  • Mixed capillary chromatographic column with shower head and preparation method thereof

Examples

Experimental program
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Effect test

Embodiment 1

[0028] Push the 0.1M HCl solution into the capillary column with a spray head with a micro-sampling pump, wash it at a flow rate of 1 μL / min for 1 hour, then inject ultrapure water into the effluent to pH 7.0 with a syringe, and then inject the 0.1M NaOH solution into the capillary column , washed at a flow rate of about 1 μL / min for 1 hour, and then washed with ultrapure water until the pH of the effluent was about 7.0.

[0029] Push 50% γ-methacryloxypropyltrimethoxysilane (γ-MAPS) / methanol solution (v / v) into the capillary, seal the end with silicone rubber, insert the nozzle end with γ-MAPS / Put the capillary in the methanol solution, seal it, and immerse the capillary in a 45°C water bath to heat for 12h. Then push out the γ-MAPS solution, rinse the capillary column with methanol solution, and dry it with nitrogen gas.

[0030] Quickly push the polymer reaction mixture solution into the capillary column with a syringe, seal the end, insert the nozzle into the casing with...

Embodiment 2

[0033] Under the exact same experimental conditions, use the automatic sample injection system to set the sample volume, and compare the effects of the packed column and the mixed column for separating the standard protease cleavage solution, see the appendix image 3 . The traditional capillary-filled chromatographic column separation and analysis of BSA trypsin digestion solution, the average coverage rate of three times is 64.36%, RSD% = 2.62; the signal intensity is 9.39E9, while the average coverage rate of the mixed capillary chromatographic column is 58.90%, RSD% = 0.81; the signal strength is 8.81E9.

Embodiment 3

[0035] Prepare mixed chromatographic columns in 3 batches according to the same method, analyze the samples of BSA trypsin digestion solution according to the same separation conditions, and record the peak capacity of each batch, select the peptide segment with a mass number of 1163.5, and record its retention The time and signal intensity are used as indicators for examining the reproducibility of the chromatographic column. The results showed that the peak capacities of the three batches were 27, 29, and 30 respectively; the retention times of the selected peptides were 44.22, 43.59, and 44.11 min, respectively. The range of the signal strength is in the order of E8.

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Abstract

The invention relates to a mixed capillary chromatographic column with a shower head and a preparation method thereof. The method comprises the following steps of: pretreating capillary tubes with different inner diameters and lengths to synthesize polymer integral materials with different lengths at the end of the shower head according to the need; filling prepared high-efficiency particle fillers by adopting a homogenate column filling method after synthesizing, and changing the type of the filler, particle size and filling length according to the requirement and synthesizing the same materials at the tail end; and compacting and ageing the materials in a high-voltage constant-current pump system by using methanol and other reagents after preparation. After evaluating the column efficiency, the prepared chromatographic column is applied to a liquid-mass combined system, and can effectively solve the problems that in a traditional filling column with the shower head, the filling particles are crushed, come out or block the shower head of the capillary chromatographic column due to over-high pressure of the capillary chromatographic column in the using process.

Description

technical field [0001] The invention belongs to the field of analytical chemistry and relates to a preparation method of a novel hybrid capillary chromatographic column with a nozzle. Background technique [0002] Liquid chromatography-mass spectrometry (LC-MS) is an analytical method that combines the separation performance of chromatography and the qualitative performance of mass spectrometry. LC-MS technology has high selectivity, sensitivity, resolution and analysis speed. In recent years, due to the continuous development and improvement of new technologies, LC-MS has become an indispensable part of modern analysis methods. It has become a powerful tool for qualitative and quantitative analysis of small molecules and biological macromolecules in complex biological samples. [0003] At present, the main problem with capillary columns used in LC-MS is that although capillary columns with tapered nozzles can significantly improve the sensitivity compared with the previou...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N30/60G01N30/56
Inventor 钱小红张养军谢晶鑫
Owner INST OF RADIATION MEDICINE ACAD OF MILITARY MEDICAL SCI OF THE PLA
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