Developments in Fast Liquid Chromatographic Analysis of Pharmaceuticals

Natishan, Theresa K.

doi:10.1080/10826076.2011.588058

Cited by 12 publications

(4 citation statements)

References 86 publications

(70 reference statements)

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“…Therefore, the HPLC method conditions were converted to UHPLC conditions, and further optimization was done on the UHPLC system using columns with 2-sub-μm particles. The small-particle technology , provides not only increased efficiency but also the ability to work at increased linear velocity without a loss of efficiency, providing both resolution and speed. , The narrower the peaks are, the easier they are to separate from each other. Also, peak height is inversely proportional to the peak width; thus, as the particle size decreases, an increase in sensitivity is obtained, since narrower peaks are taller peaks .…”

Section: Resultsmentioning

confidence: 99%

Applying QbD Principles To Develop a Generic UHPLC Method Which Facilitates Continual Improvement and Innovation Throughout the Product Lifecycle for a Commercial API

Musters¹,

Bos²,

Kellenbach³

2013

Org. Process Res. Dev.

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The application of quality-by-design (QbD) principles for new chemical entities (NCEs) is highlighted in several publications. QbD, however, is rarely applied to marketed APIs. Lifecycles of existing APIs are extending. With this extension the focus on drug safety and compliance requires up-to-date knowledge of the product and its production process as over the years expectations in this respect have shifted. We applied QbD principles in order to set up an improved control strategy for the final five steps in the production route of a steroidal contraceptive, which has been produced for over 20 years within our facilities. A generic UHPLC method was developed for the quantitative analysis of the available intermediate batches which have all resulted in compliant API at full commercial scale. On the basis of the batch results, (statistically supported) specifications are proposed to create a range of proven acceptance criteria. This approach allows the application of the historical knowledge of the drug substance and its manufacturing process gained over the years to future production by exploiting the process capability of eliminating impurities and dealing with variability in the quality of the intermediates. Furthermore, it improves the process of specification setting. Generic UHPLC methods enable rapid quantitative monitoring of quality. The use of a generic UHPLC method in combination with the setup of a side-product flow scheme improves process understanding and supports chemical entity design space development. Furthermore, the use of a generic UHPLC method for multiple intermediates also offers the possibility to perform side-product tracing on the basis of retention times. A generic UHPLC method was developed according to QbD principles to create a range of proven acceptance criteria for the assay and side-product determination for the final five steps in the production route of a contraceptive API.

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Section: Resultsmentioning

confidence: 99%

Applying QbD Principles To Develop a Generic UHPLC Method Which Facilitates Continual Improvement and Innovation Throughout the Product Lifecycle for a Commercial API

Musters¹,

Bos²,

Kellenbach³

2013

Org. Process Res. Dev.

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“…Several strategies have been used to increase the speed of LC separations, including shorter columns with new stationary phases and exploring method conditions (temperature, solvent and flow rate) to reduce analysis time ( Figure 1). Currently, columns packed with sub-2 μm particles in ultra-high performance liquid chromatography (UHPLC) systems, columns packed with partially porous particles and monolithic columns are the three main competing approaches for fast liquid chromatography (11,12). Other strategies include the use of short columns with reduced internal diameter and optimization of the method conditions to improve separation and allow higher flow rates/ linear velocity of the mobile phase.…”

Section: Fast Lc Separationsmentioning

confidence: 99%

Fast Analysis of Bioactive Compounds by Reverse Phase Liquid Chromatography

Nogueira

Rostagno

Gomes

et al. 2014

ACS Symposium Series

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The analysis of bioactive compounds in raw bioactive materials by liquid chromatography can prove to be a very difficult task and usually require extended times to adequately separate all components from such complex matrices. Currently there is a great interest in the development of new technology to improve chromatographic performance and reduce the necessary time to achieve the separation between components. Liquid chromatography has seen great improvements in the last decades, especially in stationary phase technology. New stationary phase technologies include sub2 µm particles, partially porous and porous monolithic polymers. These new packing materials are taking the chromatographic performance of separations to a much higher level. Liquid chromatography systems are also seen improvements in term of pressure limits, precision, reproducibility and overall quality of the results. The use of these advanced systems and materials allied to the adoption of carefully planned strategies under optimized conditions can produce excellent chromatographic results with speeds that were thought to be impossible a few years ago. In this context, this chapter discusses current technology available that can be explored to reduce analysis time of bioactive compounds in natural products. It also discusses the influence of most important operational parameters (column In Instrumental Methods for the Analysis and Identification of Bioactive Molecules; Jayprakasha, et al.; ACS Symposium Series; American Chemical Society: Washington, DC, 2014.temperature, mobile phase composition and flow rate/ linear velocity in the chromatographic system and how these variables can be adjusted in order to produce the greatest potential for performing separations.

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“…Working at such high pressures can also reduce the efficiency of the separations because of the frictional heating. Several reviews have been devoted to discuss the improvements in efficiency and time of analysis afforded by UPLC, UHPLC, and capillary LC compared to HPLC, − but none of them have focused on their benefits from the point of view of green analytical chemistry. , …”

Section: Columns and Stationary Phase Modificationsmentioning

confidence: 99%

Sustainable and Eco-Friendly Alternatives for Liquid Chromatographic Analysis

Olives

González‐Ruiz

Martín

2017

ACS Sustainable Chem. Eng.

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This Perspectives article covers the most relevant current strategies aimed at reducing the environmental fingerprint caused by mobile phases in liquid chromatography. Modern stationary phases, such as columns packed with core− shell particles or stationary phases allowing high-temperature separations, are discussed. Mobile-phase additives creating secondary partitioning equilibria (micelle-forming reagents, cyclodextrins, or ionic liquids) and alternatives to acetonitrile as organic solvent are critically compared in terms of separation efficacy and wastes' toxicity. Advantages of CO 2 and superheated solvents are also considered to complete the picture of the most recent developments in the field.

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Developments in Fast Liquid Chromatographic Analysis of Pharmaceuticals

Cited by 12 publications

References 86 publications

Applying QbD Principles To Develop a Generic UHPLC Method Which Facilitates Continual Improvement and Innovation Throughout the Product Lifecycle for a Commercial API

Applying QbD Principles To Develop a Generic UHPLC Method Which Facilitates Continual Improvement and Innovation Throughout the Product Lifecycle for a Commercial API

Fast Analysis of Bioactive Compounds by Reverse Phase Liquid Chromatography

Sustainable and Eco-Friendly Alternatives for Liquid Chromatographic Analysis

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