A robust, fully automated, walk-up method is reported to quantify chloride in samples using 35Cl nuclear magnetic resonance. Minimal user input is required, no standards are acquired at the time of analysis; and the submission, acquisition, processing, and production of results are seamlessly integrated within existing software. The method demonstrated good linearity with R2 = 0.999 over three orders of magnitude of analyte concentration. The results were highly independent of analyte functionality, and the stability of instrument response was sufficient that analyses of additional standards were not required for a period of several months. At a nominal sample concentration of 10 mg/ml in D2O at 400 MHz, detection and quantitation limits of 0.1 and 0.5% (w/w) were achieved in a 1-h analysis time. Robust methodology was achieved by applying a rigorous approach to method development and validation to determine and evaluate fully the time- and sample-dependent factors that affect quantitation in these measurements.
- pharmaceutical analysis
- nuclear magnetic resonance