Synthesis and application of restricted access filler having inner surface with inverting performance

An inner surface, limited access technology, which is applied to the synthesis and application of the inner surface reversed-phase limited-access packing, can solve the problems of low accuracy and precision, consumption of reagents, large sample volume, etc., and achieve good reversed-phase performance , the effect of simple operation

Inactive Publication Date: 2012-07-25
王荣
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Currently, off-line methods are usually used to pretreat biological samples, such as protein precipitation (PP); liquid-liquid extraction (LLE); solid-phase extraction (SPE); membrane extraction, etc., but these methods are cumbersome, time-consuming, and labor-intensive. , large sample volume, low accuracy and precision, and co-precipitation of the analyte and protein

Method used

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  • Synthesis and application of restricted access filler having inner surface with inverting performance
  • Synthesis and application of restricted access filler having inner surface with inverting performance
  • Synthesis and application of restricted access filler having inner surface with inverting performance

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0036] Example 1 The reverse-phase restricted-access filler on the inner surface, the restricted-access filler is a restricted-access filler with protein exclusion properties on the outer surface and reverse-phase performance on the inner surface, which has the following structural formula,

[0037]

[0038] where n=1955.

[0039] The synthesis method of the inner surface anti-phase restricted entry filler comprises the following steps:

[0040] ⑴ Synthesis of aminopropyl alkylated silica gel (APS) (see figure 1 ):

[0041] First, the porous silica gel with a particle size of 5 μm was activated by hydrochloric acid with a mass concentration of 3.65%, and then placed in a 250 mL three-necked bottle and dried in a BPZ-6033LC vacuum oven at 180 °C for 5 h to obtain activated silica gel.

[0042] Then, add activated silica gel to anhydrous toluene and reflux at a temperature of 115 ° C, and remove residual moisture azeotropically in N 2 Under protection, 3-aminopropyltriet...

Embodiment 2

[0064] Example 2 The reverse-phase restricted-access filler on the inner surface, the restricted-access filler is a restricted-access filler with protein exclusion properties on the outer surface and reverse-phase performance on the inner surface, which has the following structural formula,

[0065]

[0066] where n=500.

[0067] The synthesis method of the inner surface anti-phase restricted entry filler comprises the following steps:

[0068] ⑴ Synthesis of APS:

[0069] First, the porous silica gel with a particle size of 5 μm was activated by hydrochloric acid with a mass concentration of 3.65%, and then placed in a 250 mL three-necked bottle and dried in a BPZ-6033LC vacuum oven at 150 °C for 6 h to obtain activated silica gel.

[0070] Then, the activated silica gel was added to anhydrous toluene to reflux at a temperature of 110 ° C, and the residual moisture was removed by azeotropy in N 2 Under protection, 3-aminopropyltriethoxysilane was added, and the DF-101S...

Embodiment 3

[0083] Example 3 The reverse-phase restricted-access filler on the inner surface, the restricted-access filler is a restricted-access filler with protein exclusion properties on the outer surface and reverse-phase performance on the inner surface, which has the following structural formula,

[0084]

[0085] where n=2300.

[0086] The synthesis method of the inner surface anti-phase restricted entry filler comprises the following steps:

[0087] ⑴ Synthesis of APS:

[0088] First, the porous silica gel with a particle size of 5 μm was activated by hydrochloric acid with a mass concentration of 3.65%, and then placed in a 250 mL three-necked bottle and dried in a BPZ-6033LC vacuum oven at 200 °C for 4 h to obtain activated silica gel.

[0089] Then, add activated silica gel to anhydrous toluene and reflux at a temperature of 120°C, and remove residual moisture azeotropically under N 2 Under protection, 3-aminopropyltriethoxysilane was added, and the DF-101S collector typ...

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Abstract

The invention relates to synthesis of restricted access filler having inner surface with inverting performance, wherein the synthesis method comprises the following steps: synthesizing ammonia propyl alkylation silica gel with porous silica gel having partical size of 5 microns, and then preparing the restricted access filler with an outer surface having protein exclusion ability and the inner surface having inverting performance. Because of the synthesis routes of the invention, the key step of optionally removing the modified groups of the outer surface in the routine synthesis method of the restricted access filler is removed, at the same time, the hexylamine bonded on the inner surface is changed into the other compounds during the reaction process so as to prepare the restricted access filter with the inner surface having different functional groups according to the synthesis method. The synthesis method provided by the invention evaluates the protein exclusion ability and inverting performance performance of the restricted access filter and is used for directly performing sample injection and analysis for Propranolol serum samples.

Description

technical field [0001] The invention relates to the synthesis and application field of restricted-access fillers, in particular to the synthesis and application of an inner-surface anti-phase restricted-access filler. Background technique [0002] When biological samples (such as plasma, urine, etc.) are analyzed by HPLC, sample preparation is often the rate-limiting step and bottleneck step in the entire analysis process, which directly affects the precision and accuracy of the analysis results. Currently, off-line methods are usually used to pretreat biological samples, such as protein precipitation (PP); liquid-liquid extraction (LLE); solid-phase extraction (SPE); membrane extraction, etc., but these methods are cumbersome, time-consuming, and labor-intensive. , The sample volume is large, the accuracy and precision are not high, and there is a co-precipitation phenomenon between the analyte and the protein. In recent years, the restricted-entry fillers developed in rec...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J20/286B01J20/30C09C1/28C09C3/10C09C3/08G01N30/08
Inventor 王荣贾正平马骏谢华武晓玉杨沛
Owner 王荣
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