An estimation of the column efficiency made by analyzing tailing peak profiles

Miyabe, Kanji; Matsumoto, Yuko; Niwa, Yasumasa; Ando, Nobuho; Guiochon, Georges

doi:10.1016/j.chroma.2009.09.006

Cited by 11 publications

(17 citation statements)

References 69 publications

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“…For example, the peak asymmetry for silybin A was 1.3 ( u e =1.5 mm/s) in the monolithic column, while this value was 0.95 ( u e =1.3 mm/s) for the same analyte in the core–shell column. This fact can be explained by different radial heterogeneities of the columns 25.…”

Section: Resultsmentioning

confidence: 99%

Narrow‐bore core–shell particles and monolithic columns in the analysis of silybin diastereoisomers

Marhol

Gažák

Bednář

et al. 2011

J of Separation Science

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Two chromatographic narrow-bore columns, a novel 2.6 μm particle-packed Kinetex™ C18 core-shell (50×2.1 mm id) and monolithic Chromolith(®) FastGradient RP-18e (50×2 mm id), were evaluated for the analysis of diastereoisomers of the flavonolignans silybin and 23-O-acetylsilybin under isocratic conditions. The main advantages of the core-shell column are markedly higher efficiency (hmin =2.8 versus 5.6 for silybin A) and better peak symmetry. The Kinetex column exhibits only a slight change in the height equivalent of the theoretical plate with a higher linear velocity of the mobile phase. The monolithic column shows notably higher selectivity in terms of selectivity factor (1.21 versus 1.12) in the analysis of critical-pair of diastereoisomers (silybin A and silybin B) and enables shorter run duration (approx. twofold) together with lower backpressure. The resolution power was found to be comparable, but the Kinetex column required a higher pressure of the mobile phase that, together with the higher chance of clogging, can be a disadvantage in the separation of biological samples. Successful baseline separation of silybin diastereoisomers in real pharmaceutical sample on monolithic column was accomplished.

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Section: Resultsmentioning

confidence: 99%

Narrow‐bore core–shell particles and monolithic columns in the analysis of silybin diastereoisomers

Marhol

Gažák

Bednář

et al. 2011

J of Separation Science

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show abstract

“…It was shown earlier that changes in ν do not significantly affect the peak profiles. 26 The degree of column radial heterogeneity increases in the order (1) < (2) < (3). In the first case, the peak obtained is Gaussian, as expected.…”

Section: Resultsmentioning

confidence: 99%

“…This deviation was attributed to a numerical calculation error. 26 Apparent Column Efficiency. Figure 3b illustrates the influence of the column radial heterogeneity on the apparent column efficiency (N) calculated from the moments, µ 1 and µ 2 ′, of the peak eluting from the column.…”

Section: Resultsmentioning

confidence: 99%

“…Tailing peak profiles were numerically calculated using the equilibrium-dispersive model of chromatography, as previously explained in detail 26 and briefly indicated below. The calculations are based on the following assumptions: (1) The chromatographic process proceeds under linear isotherm conditions.…”

Section: Theorymentioning

confidence: 99%

“…It showed that the numerical method could be effective for deriving the true column efficiency at the column center from experimental profiles. However, in this earlier study, 26 we used fourth-order polynomial functions to represent the radial distributions of the flow velocity and the local column efficiency because these functions provided a proper empirical representation of the column radial heterogeneity measured. [7][8][9]13,[18][19][20] However, it is probable that the column radial heterogeneities could be better represented by other polynomial functions.…”

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confidence: 99%

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Numerical Method for the Estimation of Column Radial Heterogeneity and of the Actual Column Efficiency from Tailing Peak Profiles

Miyabe

Guiochon

2010

Anal. Chem.

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It is probably impossible to prepare high-performance liquid chromatography (HPLC) columns that have a completely homogeneous packing structure. Many reports in the literature show that the radial distributions of the mobile phase flow velocity and the local column efficiency are not flat, even in columns considered as good. A degree of radial heterogeneity seems to be a common property of all HPLC columns and an important source of peak tailing, which prevents the derivation of accurate information on chromatographic behavior from a straightforward analysis of elution peak profiles. This work reports on a numerical method developed to derive from recorded peak profiles the column efficiency at the column center, the degree of column radial heterogeneity, and the polynomial function that best represents the radial distributions of the flow velocity and the column efficiency. This numerical method was applied to two concrete examples of tailing peak profiles previously described. It was demonstrated that this numerical method is effective to estimate important parameters characterizing the radial heterogeneity of chromatographic columns.

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Chromatography: Separation Techniques in Biology

Lough

Carlile

2019

Biomolecular and Bioanalytical Techniques

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An estimation of the column efficiency made by analyzing tailing peak profiles

Cited by 11 publications

References 69 publications

Narrow‐bore core–shell particles and monolithic columns in the analysis of silybin diastereoisomers

Narrow‐bore core–shell particles and monolithic columns in the analysis of silybin diastereoisomers

Numerical Method for the Estimation of Column Radial Heterogeneity and of the Actual Column Efficiency from Tailing Peak Profiles

Chromatography: Separation Techniques in Biology

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