A generic stepwise optimization strategy for liquid chromatography electrospray ionization tandem mass spectrometry methods

Abstract

The feasibility and advantages of using sophisticated chemometric tools in combination with the execution of thoroughly planned experiments to determine experimental conditions for optimal performance of an LC-ESI-MS/MS analysis is demonstrated. A stepwise strategy is proposed, which provides a controlled optimization procedure of the chromatographic quality (in terms of separation among the sample constituents) and maximizes the mass spectrometric signal of the selected product ions. Design of experiments (DOE) and response surface methodology are applied throughout the procedure. The stepwise approach has the advantage of dealing with the different optimization criteria separately, i.e. first ensuring sufficient chromatographic separation, then maximizing the amount of precursor ion entering the mass spectrometer, and finally generating high amounts of selected product ions. The experiments are performed on a linear ion trap mass spectrometer. Retention mapping using the band-tracking model is applied during LC development, which facilitates the optimization of segmented gradients. A set of different siderophores, strong iron chelates, is used as the model substances.

Optimization and Comparison of ESI and APCI LC-MS/MS Methods: A Case Study of Irgarol 1051, Diuron, and their Degradation Products in Environmental Samples

“…Therefore, the simple application of an already published method is not always successful. There are various published optimization strategies for the development of LC-MS and tandem MS methods [23][24][25][26], and a tutorial for statistical design of experiments especially for mass spectrometry [27] offers useful guidelines. However, each analytical problem is unique and demands a particular approach.…”

Exploring analyte response in an ESI-MS system with different chemometric tools

“…Strategies that enable identification of the main effects as well as interactions among instrumental parameters and analyte physicochemical properties are essential for system understanding and response optimization [6]. In this context, the need of utilizing chemometric tools for system knowledge and for efficient experimental designs and analyses becomes apparent [6,7,11,12].…”

Ionization of tocopherols and tocotrienols in atmospheric pressure chemical ionization

“…Likewise, works describing the ion source optimization in the case of simultaneous determination of multiple tocochromanols are limited. Moreover, the majority of studies were focused on optimization of their ionization using an ESI source . To our best knowledge, only Lanina et al have described the study of various factors affecting ionization of T in APCI .…”

“…Moreover, the majority of studies were focused on optimization of their ionization using an ESI source. [23][24][25][26][27] To our best knowledge, only Lanina et al have described the study of various factors affecting ionization of T in APCI. 8 However, the authors performed individual experiments for each ionization source factor and the described methodology does not take into account interactions between factors, which might occur during ionization processes.…”