The Application Notebook
The costs associated with pharmaceutical testing are considerable, and many lab managers are seeking ways to reduce costs by reducing solvent usage and improving productivity while still using the LC instruments in their lab.
William Long, Agilent Technologies Inc., Wilmington, Delaware, USA.
The costs associated with pharmaceutical testing are considerable, and many lab managers are seeking ways to reduce costs by reducing solvent usage and improving productivity while still using the LC instruments in their lab.
Compendia methods from the United States Pharmacopeia (USP) are widely used in pharmaceutical drug product and raw materials testing. However, not all methods in the USP use modern technologies and may be more time consuming than desired for today's lab. These methods can be updated by making adjustments following the recommendations in USP chapter <621>. The ranges for adjustments are: column length, column material particle size and injection volume. While other paraneters can be adjusted according to the USP, none of those were needed to improve the throughput of this method. Modifications outside these ranges are considered changes and require revalidation of the method.
Naproxen is classified as a non-steroidal anti-inflammatory drug or NSAID and is available as a generic tablet. The USP contains a method for the analysis of Naproxen tablets which references using an L1 (C18), 5 µm column.
Poroshell 120 columns are a new LC column choice that can provide improved performance on a typical LC instrument. These columns have a 2.7 µm superficially porous particle that can provide faster analysis and high resolution in shorter columns for testing more samples in less time on existing LC instruments. The columns are available in a C18 bonded phase, a typical L1 material.
In Figure 1, a 4.6 × 150 mm, 5 µm, L1 or C18 column is used as the starting point for the method. The conditions are unchanged and both a Poroshell 120 EC-C18 4.6 × 10 mm, 2.7 µm and 4.6 × 50 mm, 2.7 µm column are compared.
Figure 1: USP method for naproxen tablets - 4.5Ã faster analysis on Poroshell 120. Common conditions: Mobile phase: 50:49:1 MeCN:H2O acetic acid; Flow rate: 1.2 mL/min; Peaks: 1 =naproxen 2 =butyrophenone.
The performance requirements of the method are exceeded when changing from the 5 µm L1 column to both of the superficially porous 2,7 µm C18 columns. The analysis on the 100 mm column is 2× faster than the original method and on the 50 mm long column the method is 4.5× faster than the original method. Either column choice improves productivity.
Laboratories performing compendia analyses with fully-porous LC columns can benefit from the increased speed, resolution and sensitivity that superficially porous, Poroshell 120 columns can provide without having to replace existing instrumentation. Faster analysis times resulting in higher throughput and greater productivity can be achieved with Poroshell 120 columns. Method adjustments to these compendia methods with shorter length columns and the smaller 2.7 µm particle size provide these improved results.
Agilent Technologies Inc.
2850 Centerville Road, Wilmington, Delaware 19808, USA
tel. +1 800 227 9770
E-mail: info_agilent@agilent.com
Analyzing Bone Proteins in Forensic Laboratories Using LC−MS/MS
November 4th 2024A recent study compared different workflows for extracting, purifying, and analyzing bone proteins using liquid chromatography with tandem mass spectrometry (LC–MS/MS), including an in-StageTip protocol previously optimized for forensic applications, and two protocols using novel suspension-trap technology (S-Trap) and different lysis solutions. LCGC International discussed this work with Noemi Procopio of the School of Law and Policing and the Research Centre for Field Archaeology and Forensic Taphonomy at the University of Central Lancashire (UK), corresponding author of the paper that resulted from this study.
AI and GenAI Applications to Help Optimize Purification and Yield of Antibodies From Plasma
October 31st 2024Deriving antibodies from plasma products involves several steps, typically starting from the collection of plasma and ending with the purification of the desired antibodies. These are: plasma collection; plasma pooling; fractionation; antibody purification; concentration and formulation; quality control; and packaging and storage. This process results in a purified antibody product that can be used for therapeutic purposes, diagnostic tests, or research. Each step is critical to ensure the safety, efficacy, and quality of the final product. Applications of AI/GenAI in many of these steps can significantly help in the optimization of purification and yield of the desired antibodies. Some specific use-cases are: selecting and optimizing plasma units for optimized plasma pooling; GenAI solution for enterprise search on internal knowledge portal; analysing and optimizing production batch profitability, inventory, yields; monitoring production batch key performance indicators for outlier identification; monitoring production equipment to predict maintenance events; and reducing quality control laboratory testing turnaround time.
Profiling Volatile Organic Compounds in Whisky with GC×GC–MS
November 1st 2024Researchers from Austria, Greece, and Italy conducted a study to analyze volatile organic compounds (VOCs) present in Irish and Scotch whiskys using solid-phase microextraction (SPME) Arrow with comprehensive two-dimensional gas chromatography coupled to mass spectrometry (GC×GC–MS) to examine the organoleptic characteristics that influence the taste of spirits.