Performance Comparison Between Monolithic, Core-Shell, and Totally Porous Particulate Columns for Application in Greener and Faster Chromatography

2018 ◽  
Vol 101 (6) ◽  
pp. 1985-1992 ◽  
Author(s):  
Adel Ehab Ibrahim ◽  
Hisham Hashem ◽  
Hanaa Saleh ◽  
Magda Elhenawee

Abstract Background: The introduction of monolithic rods and core-shell particles as new morphologies of packing materials different from the conventional totally porous particles resulted in a leap forward for performance in LC. Meanwhile, environmental safety has become increasingly important in many areas, especially in industry and research laboratories. Objective: This study compared the efficiencies of commercially available columns of different lengths and diameters when greener chromatographic conditions were utilized. The main purpose of this study is to help practitioners select the most appropriate stationary phase for faster and greener analysis. Methods: The three types of stationary phases were compared in terms of separation efficiency, number of theoretical plates, peak shape, selectivity, resolution, analysis time, mobile phase consideration, and permeability using six drug molecules. Results: Results indicated that core-shell and monolithic stationary phases had superiority over the conventional totally porous particles in terms of efficiency and speed of analysis. Monolithic rods had lower column backpressure and higher permeability, so they are more suitable for higher mobile phase flow rates and viscosities. However, core-shell particles provided enhanced peak shapes and number of theoretical plates. Conclusions: The choice will depend on the main purpose of analysis and the composition of the mobile phase. Compromise must be made to obtain the best trade-off between separation efficiency and analysis speed. Highlights: This study is the first to consider green chromatography concepts for the selection of the best stationary phase of new morphologies.

2018 ◽  
Vol 46 (1) ◽  
pp. 39-42
Author(s):  
Dana Moravcová ◽  
Josef Planeta

Abstract The monolithic capillary columns (0.1 mm x 150 mm) prepared by the acidic hydrolysis of tetramethoxysilane (TMOS) in the presence of polyethylene glycol (PEG) and urea were modified by zwitterionic stationary phases and evaluated under HILIC separation conditions by employing a mixture containing nucleosides and nucleotides. The polymeric layer of zwitterions did not affect the high separation efficiency of the original silica monolith. The prepared zwitterionic columns exhibited high separation efficiencies in a range 61,000-289,000 theoretical plates/m for a 2- methacryloyloxyethyl phosphorylcholine-based stationary phase and in a range 59,000-135,000 theoretical plates/m for a [2-(methacryloyloxy)ethyl]dimethyl-(3-sulfopropyl)ammonium hydroxide-based stationary phase under optimal separation conditions. The grafted layer of zwitterions on the silica monolithic surface also significantly improved the separation selectivity to compounds of interest


2016 ◽  
Vol 2016 ◽  
pp. 1-12 ◽  
Author(s):  
Christophe Waterlot ◽  
Anaïs Goulas

Effects of temperature on the reversed-phase chromatographic behavior of PAHs were investigated on three columns. The first was the recent C18column (250 mm × 4.6 mm) packed with 5 µm core-shell particles while the others were more conventional C18columns (250 mm × 4.6 mm) packed with fully porous particles. Among the 16 PAHs studied, special attention has been paid to two pairs of PAHs, fluorene/acenaphthene and chrysene/benzo[a]anthracene, which often present coeluting problems. Due to the low surface area of the core-shell particles, lowest retention time of each PAH was highlighted and effects of the temperature on the separation of PAHs were negligible in regard to those using columns packed with fully porous particles. For each PAH studied, it was demonstrated that peaks were symmetrical and may be considered as Gaussian peaks when the column packed with core-shell particle was employed. In the best condition, the separation of PAHs was conducted at 16°C under very low pressure values (670–950 psi = 46–65 bars). Depending on PAHs, the limit of detection ranged from 0.88 to 9.16 μg L−1. Analysis of spiked acetonitrile samples with PAHs at 10 and 50 µg L−1and tap water at 10 µg L−1gave very good recoveries (94%–109.3%) and high precision (1.1%–3.5%).


2013 ◽  
Vol 76 (15-16) ◽  
pp. 921-927 ◽  
Author(s):  
Takafumi Kimura ◽  
Hatsuichi Ohta ◽  
Koichi Wada ◽  
Kiyokatsu Jinno ◽  
Ikuo Ueta ◽  
...  

2021 ◽  
Vol 17 (3) ◽  
pp. 439-446
Author(s):  
Hongjun Xia ◽  
Huaiming Wang ◽  
Jianshan Wang ◽  
Lin Wang ◽  
Lin Jin ◽  
...  

As it is difficult to prevent secondary nucleation and agglomeration during the preparation of core–shell silica microspheres, these issues have been successfully resolved in this study using template-dissolution-induced redeposition. The non-porous particles are transformed into core–shell silica microspheres (CSSMs) in the presence of cetyltrimethylammonium bromide and octyltrimethylammonium bromide under basic conditions. The shell thickness and pore sizes of the CSSMs are controlled by adjusting the etching time and molar ratio of the template, respectively. The CSSMs are modified using octadecyltrimethylammonium chloride to separate the mixture of alkyl benzenes, and a high column separation efficiency is achieved within two minutes. The CSSMs are used for the separation and analysis of proteins and the digests of bovine serum albumin. The chromatographic column packed with core–shell particles affords a significantly higher separation efficiency than the commercial column. Therefore, as a chromatographic stationary phase, these core–shell particles can potentially be used for the fast separation of proteins, small solutes, and complex samples.


2016 ◽  
Vol 2016 ◽  
pp. 1-9 ◽  
Author(s):  
Raffaella Preti

The increased separation efficiency provided by the new technology of column packed with core-shell particles in high-performance liquid chromatography (HPLC) has resulted in their widespread diffusion in several analytical fields: from pharmaceutical, biological, environmental, and toxicological. The present paper presents their most recent applications in food analysis. Their use has proved to be particularly advantageous for the determination of compounds at trace levels or when a large amount of samples must be analyzed fast using reliable and solvent-saving apparatus. The literature hereby described shows how the outstanding performances provided by core-shell particles column on a traditional HPLC instruments are comparable to those obtained with a costly UHPLC instrumentation, making this novel column a promising key tool in food analysis.


2019 ◽  
Vol 15 (2) ◽  
pp. 200-209
Author(s):  
Canyu Yang ◽  
Ji Li ◽  
Yanyun Yao ◽  
Chen Qing ◽  
Baochun Shen

Background: Cinacalcet is one of the second-generation calcimimetics which consists of a chiral center. The pharmacological effect of R-cinacalcet is 1000 times greater than that of the Scinacalcet. As mentioned in many literatures, 1-(1-naphthyl)ethylamine is used as the starting material for the synthesis of cinacalcet. The absolute structure of cinacalcet is influenced by the starting materials. Methods: We present the chiral separation of cinacalcet and its starting material, 1-(1-naphthyl) ethylamine along with one of its intermediates, N-(1-(naphthalen-1-yl) ethyl)-3- (3-(trifluoromethyl) phenyl) propanamide by high-performance liquid chromatography with chiral stationary phase and chiral mobile phase additives. Results: On vancomycin and cellulose tri 3,5-dimethylphenylcarbamate) chiral stationary phase, cinacalcet and 1-(1-naphthyl)ethylamine achieved enantioseparation under normal phase with addition of triethylamine additives, respectively. Meanwhile, 1-(1-naphthyl)ethylamine and N-(1-(naphthalen-1- yl)ethyl)-3-(3-(trifluoromethyl) phenyl) propanamide achieved enantioseparation on 1-napthalene vancomycin chiral stationary phase using D-tartaric acid, diethyl L-tartrate and diethyl D-tartrate as chiral mobile phase additives. Conclusion: The chiral recognition in our experiment was based on the hydrogen-bonding, dipoledipole and π-π interactions among the solutes, chiral stationary phases and chiral mobile phase additives. In addition, the space adaptability of chiral stationary phases also affected the separation efficacy.


Chirality ◽  
2018 ◽  
Vol 30 (9) ◽  
pp. 1067-1078 ◽  
Author(s):  
Garrett Hellinghausen ◽  
Diego A. Lopez ◽  
Jauh T. Lee ◽  
Yadi Wang ◽  
Choyce A. Weatherly ◽  
...  

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