Looking for breakthrough ideas for innovation challenges? Try Patsnap Eureka!

A kind of polar liquid chromatography filler and preparation method thereof

A high-performance liquid chromatography and polar technology, which is applied in the field of polar liquid chromatography packing and its preparation, can solve the problems of poor reproducibility of two-step synthesis, poor acid and alkali resistance of packing, and poor batch reproducibility, etc., achieving Excellent selectivity and resolution, strong separation ability, effect of eliminating influence

Inactive Publication Date: 2016-08-03
FOURTH MILITARY MEDICAL UNIVERSITY
View PDF3 Cites 1 Cited by
  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Buszewski et al. (J.Chromatogr.A1994,763,11) prepared an amide-type charge-shielding bonded stationary phase for the separation of basic compounds, but the reproducibility of the two-step synthesis method is poor, and the unreacted amino group is easily separated from the analyte Performs ion exchange, causing peak tailing
The main disadvantages of the prior art are: 1. There are many side reactions in the two-step bonding process; 2. The reproducibility between batches is poor; 3. The filler has poor acid and alkali resistance

Method used

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
View more

Image

Smart Image Click on the blue labels to locate them in the text.
Viewing Examples
Smart Image
  • A kind of polar liquid chromatography filler and preparation method thereof
  • A kind of polar liquid chromatography filler and preparation method thereof
  • A kind of polar liquid chromatography filler and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0028] The synthesis of embodiment 1 silane and polar chromatography stationary phase

[0029] 1.1 Preparation of Undecylglycine

[0030]

[0031] Add CH to a 250mL three-necked flask 2 Cl 2 (50 mL), undecyl chloride (4.49 g) and triethylamine (5 mL), vigorously stirred in an ice bath, and CH containing glycine (1.5 g) was added dropwise 2 Cl 2 solution (20 ml). After the dropwise addition was completed, the reaction was stirred at room temperature for 2 hours. The crude product was purified by column chromatography using ethyl acetate / petroleum ether (3:1) as the eluent to obtain a colorless oily liquid product (4.53 g). 1 HNMR (500MHz, CDCl 3 )δ0.84(t,3H),1.29(m,14H),1.58(m,2H),2.15(m,2H),4.16(s,2H).Calc.C%64.16,H%10.36,N% 5.76; Found C% 64.10, H% 10.38, N% 5.71.

[0032] 1.2 Preparation of silanes containing double amide bonds

[0033]

[0034] Add undecylglycine (2.4 g), N,N’-dicyclohexylcarbodiimide (2.1 g), 4-dimethylaminopyridine (70 mg) and CH 2 Cl 2(1...

Embodiment 2

[0041] The following series of polar high performance liquid chromatography fillers containing double amide bonds were synthesized by a synthesis method similar to that of Example 1.

[0042]

[0043] The structure of the above-mentioned synthesized substance was confirmed by infrared, NMR and elemental analysis.

Embodiment 3

[0044] Embodiment 3 chromatographic column performance evaluation

[0045] 3.1 Packing of analytical column

[0046] The filler prepared in Example 1 is filled in a 150x4.6mmI.D. stainless steel column tube by the homogenization method, and the filling pressure is preferably 40-80MPa. The resulting column is used to separate mixture samples.

[0047] 3.2 Engelhardt test

[0048] Using the chromatographic column prepared in Example 3.1, 1 thiourea, 2 aniline, 3o-, m-, p-toluidine, 4 phenol, 5N, N-dimethylaniline, 6 ethyl benzoate, 7 toluene, 8 ethylbenzene mixture, figure 1 for its chromatogram. The chromatographic conditions are as follows: mobile phase, methanol:water=55:45 (v / v); flow rate, 1mL / min; column temperature, 25 0 C; detection wavelength, UV254nm.

[0049] 3.3 Stability test

[0050] With the chromatographic column prepared in Example 3.1, the stability of the chromatographic column of the present invention at different pHs was measured ( figure 2 ). The ...

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
Login to View More

PUM

PropertyMeasurementUnit
particle diameteraaaaaaaaaa
specific surface areaaaaaaaaaaa
Login to View More

Abstract

The invention discloses a polar high-performance liquid chromatography filler containing double amide bonds. Its general chemical structure is as follows, wherein R1 is a C1-C20 alkyl group, R2 is a C1-C8 alkyl group or phenyl group, a 0, 1, 2, X is halogen, alkoxy, acyloxy or amine. The invention utilizes a novel polar double amide bond functional group as the bonded phase on the surface of the silica gel, which can form a hydrogen bond or ion pair with the residual silanol on the silica gel matrix, better shield the activity of the silanol, and eliminate the influence of the residual silanol. Compared with traditional C18 chromatographic columns, these new chromatographic stationary phases have better selectivity and resolution, high column efficiency and wide application range.

Description

technical field [0001] The invention belongs to the technical field of preparation of high performance liquid chromatography separation materials, in particular to a polar liquid chromatography filler and a preparation method thereof, which is suitable for separating polar and basic compounds and is used in organic synthesis, food, environment and pharmaceutical industries Separation and purification of multi-component mixtures. Background technique [0002] High-performance liquid chromatography (HPLC) is an efficient and rapid separation and analysis technology developed in the 1970s. Commonly used separation and analysis methods. The basic requirement of chromatographic analysis is to achieve the separation of the components of the mixture, and the essence of the separation is based on the difference in the interaction between the analyzed solute and the mobile phase and stationary phase. Among them, the development of high-selectivity stationary phase is the core of se...

Claims

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
Login to View More

Application Information

Patent Timeline
no application Login to View More
Patent Type & Authority Patents(China)
IPC IPC(8): B01J20/286B01J20/30G01N30/60
CPCB01D15/305B01D15/322B01D15/325B01D15/327B01J20/28004B01J20/28059B01J20/28061B01J20/28083B01J20/283B01J20/286B01J20/291B01J20/3204B01J20/3227B01J20/3259B01J20/3261B01J2220/54B01J2220/58
Inventor 文爱东孙晓莉王海波贾艳艳
Owner FOURTH MILITARY MEDICAL UNIVERSITY
Who we serve
  • R&D Engineer
  • R&D Manager
  • IP Professional
Why Patsnap Eureka
  • Industry Leading Data Capabilities
  • Powerful AI technology
  • Patent DNA Extraction
Social media
Patsnap Eureka Blog
Learn More
PatSnap group products

Browse by: Latest US Patents, China's latest patents, Technical Efficacy Thesaurus, Application Domain, Technology Topic, Popular Technical Reports.

© 2024 PatSnap. All rights reserved.Legal|Privacy policy|Modern Slavery Act Transparency Statement|Sitemap|About US| Contact US: help@patsnap.com