The following question and answer were taken from LCGC Europe's "CE Currents" column (1).
The following question and answer were taken from LCGC Europe’s “CE Currents” column (1).
What do I need to cover during CE method validation?
This largely depends on the final optimized diluent that is included in the method. For example, if the final method states 5 mM phosphate pH 2.3 as the diluent — it may be appropriate to assess diluent in the range 4–6 mM and pH 2.1–2.5 to gain confidence in performance and allow some flexibility during sample diluent preparation. System suitability samples should be run prepared in diluents covering the ranges being assessed. Once the limits have been scientifically proven to be acceptable then they can be included in the method, for example, to prepare samples in 4–6 mM phosphate at pH 2.1–2.5.
Robustness experiments should be conducted using appropriate samples and standards to test the impact of diluent composition variations and to determine operating limits.
Attention to sample stability in the optimized dissolving solvent would need to be tested to experimentally determine a shelf-life for samples.
Reference
(1) K. Altria, LCGC Europe, April 2008.
Best of the Week: Food Analysis, Chemical Migration in Plastic Bottles, STEM Researcher of the Year
December 20th 2024Top articles published this week include the launch of our “From Lab to Table” content series, a Q&A interview about using liquid chromatography–high-resolution mass spectrometry (LC–HRMS) to assess chemical hazards in plastic bottles, and a piece recognizing Brett Paull for being named Tasmanian STEM Researcher of the Year.
Using LC-MS/MS to Measure Testosterone in Dried Blood Spots
December 19th 2024Testosterone measurements are typically performed using serum or plasma, but this presents several logistical challenges, especially for sample collection, storage, and transport. In a recently published article, Yehudah Gruenstein of the University of Miami explored key insights gained from dried blood spot assay validation for testosterone measurement.
Determination of Pharmaceuticals by Capillary HPLC-MS/MS (Dec 2024)
December 19th 2024This application note demonstrates the use of a compact portable capillary liquid chromatograph, the Axcend Focus LC, coupled to an Agilent Ultivo triple quadrupole mass spectrometer for quantitative analysis of pharmaceutical drugs in model aqueous samples.