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Polar liquid chromatogram filler and preparation method thereof

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

Inactive Publication Date: 2013-09-18
FOURTH MILITARY MEDICAL UNIVERSITY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Buszewski et al. (J. Chromatogr. A 1994, 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 was poor, and the unreacted amino groups were easily separated from the analysis. Ion-exchange of substances, resulting in chromatographic 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

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  • Polar liquid chromatogram filler and preparation method thereof
  • Polar liquid chromatogram filler and preparation method thereof
  • Polar liquid chromatogram 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 250 mL 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 (500 MHz, CDCl 3 ) δ 0.84 (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] Undecylglycine (2.4 g) was added to the three-necked flask, N,N'- Dicyclohexylcarbodiim...

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] Example 3 Chromatographic column performance evaluation

[0045] 3.1 Packing of analytical column

[0046] The filler prepared in Example 1 is filled in a 150 x 4.6 mm I.D. stainless steel column tube by the homogenization method, and the filling pressure is preferably 40-80 MPa. The resulting column is used to separate mixture samples.

[0047] 3.2 Engelhardt test

[0048] With the chromatographic column prepared in embodiment 3.1, 1 thiourea, 2 aniline, 3 o-, m-, p - Toluidine, 4 phenol, 5 N,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, 1 mL / min; column temperature, 25 0 C; Detection wavelength, UV 254 nm.

[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 ( ...

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Abstract

The invention discloses polar liquid chromatogram filler comprising double amido bonds. The chemical structural formula of the filer is shown in the specification, in which R1 is C1-20 alkyl, R2 is C1-8 alkyl or phenyl, a is 0, 1, 2, and X is halogen, alkoxyl, acyloxyl or amido. The filler provided by the invention can form a hydrogen bond or an ion pair with residual silicon hydroxyl on a silica-gel substrate by means of a novel polar double amido bond functional group as a silica-gel surface bonded phase, so that the activity of silicon hydroxyl is better shielded and the influence of residual silicon hydroxyl is eliminated. Compared with conventional C18 chromatographic column, the novel chromatographic fixed phases have more excellent selectivity and separation degree, so that the filler is high in column efficiency and wide in 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

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Application Information

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Patent Type & Authority Applications(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
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