Chromatography

Core-shell Phases (Part 2 of 2)

Core-shell technology

In core-shell technology a sol-gel process is used to build a shell of porous silica around a core of solid silicon dioxide. Depending on the manufacturer, a 2.7 (or 2.6) µm core-shell particle has a core of 1,7 (or 1,9) µm and a porous shell of 0.5 (or 0.35) µm, respectively. The diffusion path of the mobile phase through the porous layer (mean diffusion path about 0.5 µm) is shortened considerably compared to fully porous 3 µm particles (mean diffusion path about 1.5 µm).

core shell phases 3Shorter diffusion paths allow a rapid mass transfer of the analyte between the stationary phase (core-shell particle) and the mobile phase (eluent). In this case term C of the van Deemter equation is a function of the “effective particle size“ which is determined by the porous shell and thus smaller than for totally porous particles. A small term C enables the required low plate height h even at high velocities u. Short diffusion paths also allow high flow velocities for rapid analyses without peak broadening.

Term A, the so-called Eddy diffusion, is a function of the particle size, too. It is discussed, whether the smaller size of the core-shell particles and a narrow particle size distribution decrease the Eddy diffusion, resulting in a smaller peak width. Anyway, a narrow particle size distribution results in a homogeneous and thus stable packing.

core shell phases 4

 

 

 

 

 

 

 

 

 

 

The van Deemter plots show that the minimum plate height h of the 3 µm totally porous phase is relatively high and at a low flow velocity. As expected, the sub-2 µm phase (1,8 µm) shows low plate heights also for higher velocities. Most of the core-shell phases investigated exhibit the benefit of even lower h values at comparably high velocities. The respective minima of effective plate height are at relatively high linear velocities.

core shell phases 5

 

 

 

 

 

 

 

 

 

Considering the pressure drop, the benefits of core-shell phases become even more apparent. Even for high flow velocities pressures are only slightly higher than for the 3 µm phase, while the pressure increases considerably for the sub-2 µm phase (1.8 µm).

Thus, use of core-shell phases allows better resolution combined with lower back pressure and shorter analysis time.

core shell phases 6

 NUCLEOSHELL core-shell phases

The novel NUCLEOSHELL phases from MACHEREY-NAGEL are based on the beneficial core-shell technology. They consist of a solid core of silicon dioxide of 1.7 µm diameter and a homogeneous 0.5 µm shell of porous silica resulting in a particle size of 2.7 µm. A comparison of the theoretical column efficiency with totally porous silica phases shows, that resolution is increased and analysis time is reduced considerably.

core shell phases 7

 

 

 

 

Two modifications are available based on core-shell technology: an octadecyl modification (RP 18) and an ammonium – sulfonic acid modification (HILIC).

NUCLEOSHELL RP 18 combines the advantages of rapid and efficient HPLC with the wide applicability of a RP 18 phase. The Sorbtech application database contains numerous separation examples. Due to the state-of-the-art base deactivation, suitability for LC/MS and the high pH stability (1–11) almost all analytical RP 18 methods from porous silica columns can be transferred.

Especially for the analysis of highly polar analytes (e.g., nucleobases, nucleotides, melamine, amino acids, catecholamines) NUCLEOSHELL HILIC is recommended. This phase too can be used with LC/MS detection.

Conclusion

Core-shell technology enables HPLC phases with highest efficiency concerning resolution and analysis time at moderate pressures. The new NUCLEOSHELL RP 18 utilizes this advantage for analytical RP 18 applications on all HPLC instruments; NUCLEOSHELL HILIC is recommended for polar analytes.

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Core-shell Phases (Part 1 of 2)

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Economical Preparative HPLC (Part 1 of 2)

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