Practical comparison of 2.7μm fused-core silica particles and porous sub-2μm particles for fast separations in pharmaceutical process development

Abrahim, Ahmed; Al‐Sayah, Mohammad A.; Skrdla, Peter J.; Bereznitski, Y.; Chen, Yadan; Wu, Nan

doi:10.1016/j.jpba.2009.08.023

Cited by 76 publications

(41 citation statements)

References 25 publications

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“…Ascentis ® Express column, which is packed with unique 2.7-µm fused-core particles, 23 showed the best performance, i.e., better resolution and peak sharpness with a low back pressure compared to other conventional particulate columns. [24][25][26] Accordingly, almost all constituents of P. koreana extract, including the four triterpenoid saponins, were fairly well resolved within 26 min of elution ( Figure 5). …”

Section: Resultsmentioning

confidence: 94%

Simultaneous Determination of Triterpenoid Saponins from Pulsatilla koreana using High Performance Liquid Chromatography Coupled with a Charged Aerosol Detector (HPLC-CAD)

Yeom¹,

Suh²,

Youm³

et al. 2010

Bulletin of the Korean Chemical Society

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Several triterpenoid saponins from root of Pulsatilla koreana Nakai (Ranunculaceae) were studied and their biological activities were reported. It is difficult to analyze triterpenoid saponins using HPLC-UV due to the lack of chromophores. So, evaporative light scattering detection (ELSD) is used as a valuable alternative to UV detection. More recently, a charged aerosol detection (CAD) has been developed to improve the sensitivity and reproducibility of ELSD. In this study, we developed and validated a novel method of high performance liquid chromatography coupled with a charged aerosol detector for the simultaneous determination of four triterpenoid saponins: pulsatilloside E, pulsatilla saponin H, anemoside B4 and cussosaponin C. Analytes were separated by the Supelco Ascentis ® Express C18 column (4.6 mm × 150 mm, 2.7 µm) with gradient elution of methanol and water at a flow rate of 0.8 mL/min at 30 o C. We examined various factors that could affect the sensitivity of the detectors, including various concentrations of additives, the pH of the mobile phase, and the CAD range. Linear calibration curves were obtained within the concentration ranges of 2 -200 µg/mL for pulsatilloside E, anemoside B4 and cussosaponin C, and 5 -500 µg/mL for pulsatilla saponin H with correlation coefficient (R 2 ) greater than 0.995. The limit of detection (LOD) and quantification (LOQ) were 0.04 -0.2 and 2 -5 µg/mL, respectively. The validity of the developed HPLC-CAD method was confirmed by satisfactory values of linearity, intra-and inter-day accuracy and precision. This method could be successfully applied to quality evaluation, quality control and monitoring of Pulsatilla koreana.

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Section: Resultsmentioning

confidence: 94%

Simultaneous Determination of Triterpenoid Saponins from Pulsatilla koreana using High Performance Liquid Chromatography Coupled with a Charged Aerosol Detector (HPLC-CAD)

Yeom¹,

Suh²,

Youm³

et al. 2010

Bulletin of the Korean Chemical Society

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“…Shell particles are a relatively recent trend in chromatographic separation, but several pharmaceutical-bioanalytical [105][106][107][108][109][110][111][112][113][114][115][116][117][118], food analytical [119][120][121][122][123][124][125][126][127][128][129], environmental [130][131][132][133][134] and multidimensional [135][136][137] separations can be found in the literature. Very recently, new commercially available wide-pore stationary phases demonstrate exceptional efficiency for protein separations [138][139][140].…”

Section: Superficially Porous Particlesmentioning

confidence: 99%

Evolution and Current Trends in Liquid and Supercritical Fluid Chromatography

Fekete¹,

Perrenoud²,

Guillarme

2014

CCHG

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Abstract:The current trend in high performance liquid chromatography (HPLC) tends toward the achievement of higher separation efficiency and shorter analysis time. Indeed, better performance in LC has become increasingly important in recent years mainly driven by the challenges of either analyzing more complex samples or increasing the numbers of samples per time unit. In the recent development of particle technology, the use of fully porous sub-2 m particles and sub-3 m shell particles have received considerable attention. Beside packed columns, the new generation of silica-based monolithic columns also offers very high separation power. However, to take full advantage of these innovative phases, the chromatographic system has also to be drastically optimized in terms of upper pressure limit and system volume.This revolution in column technology now spreads and covers several modes of liquid chromatography such as reversedphase liquid chromatography (RPLC), hydrophilic interaction liquid chromatography (HILIC), or even supercritical fluid chromatography (SFC). The HILIC and SFC, which can be considered as alternative modes of chromatography, could also be useful to extend the applicability of chromatography towards the analysis of very hydrophilic and lipophilic compounds, respectively.The present review gives an insight about the theory behind the success of current column technology and presents a summary of latest applications, using various modes of one-dimensional chromatography (RPLC, HILIC, SFC). This paper also shows that theoretically expected column efficiency could sometimes be compromised in practical work especially in the case of narrow bore columns.

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“…2.6-2.7 micron fusedcore columns generate backpressures similar to those of a standard fully porous-3 µm column. The great advantage of fused core material is that these columns allow achievement of UHPLC-like resolution, without dramatic increase of the backpressure, therefore negating the necessity to purchase a UPLC/UHPLC system [1,2]. The relatively low pressure generated by fused core particles and the thin (about 0.5 µm) layer of stationary phase allows operation of fast flow rates without the loss of resolution by using standard HPLC equipment.…”

Section: Introduction Fused Core Particle In 1d Chromatographymentioning

confidence: 99%

Application of Fused-Core Particle Column in Two Dimensional Reversed Phase - Reversed Phase LC/MS Analysis of Biological Samples. Impact of Extra-Column Volume

Rogatsky¹

2012

J Chromat Separation Techniq

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We demonstrate successful applicability of fused-core column in analysis of biological samples (diluted urine and SPE-pre-purified plasma or serum) using 2 dimensional chromatography. Implementation of fused-core material in the second dimension of 2D chromatographic platform allowed improving S/N above 4 fold in comparison to traditional porous C18 column. Sample load onto the first dimension (5 µm) eliminates limitations of sample volume to be injected. The main limitation factor of the fused-core material-low loading capacity was overcome by using 2D chromatography. We emphasize importance of reduction of post-column (extra column) volume in LC/MS applications utilizing fused-core columns.

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Practical comparison of 2.7μm fused-core silica particles and porous sub-2μm particles for fast separations in pharmaceutical process development

Cited by 76 publications

References 25 publications

Simultaneous Determination of Triterpenoid Saponins from Pulsatilla koreana using High Performance Liquid Chromatography Coupled with a Charged Aerosol Detector (HPLC-CAD)

Simultaneous Determination of Triterpenoid Saponins from Pulsatilla koreana using High Performance Liquid Chromatography Coupled with a Charged Aerosol Detector (HPLC-CAD)

Evolution and Current Trends in Liquid and Supercritical Fluid Chromatography

Application of Fused-Core Particle Column in Two Dimensional Reversed Phase - Reversed Phase LC/MS Analysis of Biological Samples. Impact of Extra-Column Volume

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