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Supercritical/sub-critical fluid blocking method of HPLC (High Performance Liquid Chromatography) reversed phase bonded stationary phase

A high-performance liquid chromatography and subcritical fluid technology, applied in chemical instruments and methods, and other chemical processes, to achieve the effects of reducing pollution, mild process reaction conditions, and realizing semi-automation

Inactive Publication Date: 2015-08-19
WUHAN CHROM MATRIX BIOTECH CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

In fact, capping under solid-liquid reflux is a dead end no matter what catalyst and capping reagent is used

Method used

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  • Supercritical/sub-critical fluid blocking method of HPLC (High Performance Liquid Chromatography) reversed phase bonded stationary phase
  • Supercritical/sub-critical fluid blocking method of HPLC (High Performance Liquid Chromatography) reversed phase bonded stationary phase
  • Supercritical/sub-critical fluid blocking method of HPLC (High Performance Liquid Chromatography) reversed phase bonded stationary phase

Examples

Experimental program
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Effect test

Embodiment 1

[0046] Example 1: 5 μm C18 bonded phase supercritical fluid capping

[0047] Traditional solid-liquid reflux capping method: Japan Daiso Company 5 μm B-type spherical silica gel and silane reagent octadecyldimethylchlorosilane are used as raw materials, toluene is used as solvent, imidazole and pyridine are used as catalysts, reflux at toluene reflux temperature with nitrogen protection for 24 hours, and C18 bonded phase is obtained after washing. Technical parameters: specific surface area 300m 2 / g, bonding density 3.2μmol / m 2 .

[0048] 100g C18 bonded phase uses trimethylchlorosilane as the end-capping reagent, and 1,1,1,3,3,3-hexamethyldisilazimide, N,N-dimethyltrimethylsilylamine, etc. As a catalyst, it was refluxed for 24 hours at the reflux temperature of toluene with nitrogen protection. After the reaction, use toluene, dichloromethane, acetonitrile, methanol and water (50:50), wash with acetone in sequence, dry under nitrogen protection at 80°C, and use after co...

Embodiment 2

[0050] Example 2: Surface Charge Titration

[0051] Surface charge titration and Zeta potential are two of the most important surface characterization techniques in the field of colloid and interface science. Titration method: 10 grams of chromatographic bonded phase is placed in the potentiometric titration chamber, with 10mM sodium chloride (80%) and methanol (20%) as the liquid phase, with 0.1M hydrochloric acid to adjust the pH value to 3.0, from pH value 3.0 in nitrogen Under protection, it was titrated to pH8 with 0.1M NaOH, back-titrated to pH3.0 with 0.1M hydrochloric acid, and again titrated to pH8.0 with 0.1M NaOH.

[0052] The raw potentiometric titration data is transferred to the computer and converted into a pH-surface charge curve.

[0053] The pH-surface charge curve as a new dimension test platform can clearly reveal the surface charge of many reversed phase chromatography products on the market.

[0054] Type B spherical silica itself has 8μmol / m 2 Of the ...

Embodiment 3

[0059] Example 3: Zeta Potential

[0060] The pH-surface charge density curve alone makes it difficult to determine the isoelectric point (i.e.p) of a bonded phase. This is accompanied by a Zeta potential measurement. Zeta potential of Supelco HS C18 and Supelco ABZ Plus as image 3 shown.

[0061] The isoelectric point of Supelco HS C18 is at pH2.7, which is similar to that of silica gel itself. Supelco ABZ Plus due to residual NH 2 functional group, the isoelectric point shifts to pH4.4.

[0062] Since the supercritical fluid capping seals the active silanol groups to the greatest extent, the surface charge density of Novel C18 is almost zero, and the surface charge cannot be observed by Zeta potential measurement.

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Abstract

The invention discloses a supercritical / sub-critical water blocking method of HPLC (High Performance Liquid Chromatography) reversed phase bonded stationary phase, which comprises the steps of using carbon dioxide supercritical fluid and / or carbon dioxide sub-critical fluid as a carrier, bring a blocking reagent and a catalyst into a supercritical / sub-critical fluid reactor loaded with silica gel reversed phase bonded stationary phase, and carrying out blocking reaction under a closed condition. According to the method, residual active silanol groups can be thoroughly closed, and lyophobic reversed phase bonded stationary phase with complete neutral charge is produced; no residual active silanol groups exchanges side effects with alkali compound cations, so that alkali compound has a very symmetrical peak shape, and the retention time and mechanism fully follow the order from low to high of hydrophobicity of the compound. The method has the advantages that the reaction condition is mild, the reversed phase bonded stationary phase has no damage, the life of a chromatographic column is long, the repeatability of production batches is very good, the use amount of a toxic organic solvent, such as methylbenzene, is minimized, the pollution to the environment is reduced to the greatest extent, and the process continuity and semi-automatization can be realized.

Description

technical field [0001] The invention relates to a super / subcritical fluid end-capping method for a reversed-phase bonded phase of high performance liquid chromatography. Background technique [0002] High performance reversed-phase liquid chromatography columns represented by C18 have been described as the heart of drug discovery, development, and method validation (validation), and high performance reversed-phase liquid chromatography columns are also widely used in drug metabolism and kinetics, life sciences , medical health, biological analysis and testing, drug and doping testing, food safety analysis, environmental analysis, military, homeland security and other fields. High performance reversed-phase liquid chromatography preparative column is also one of the most important separation and purification technologies. [0003] Routine HPLC method development almost always starts with C18, with reversed-phase chromatography accounting for more than 80% of applications. N...

Claims

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Application Information

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IPC IPC(8): B01J20/286B01J20/30
Inventor 杨育晖
Owner WUHAN CHROM MATRIX BIOTECH CO LTD
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