Screening ionisation and chromatography conditions for quantitative LC/MS methods

Sillén, Henrik; Magnell, Niklas

doi:10.1016/j.jchromb.2009.08.049

Cited by 8 publications

(4 citation statements)

References 26 publications

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“…19 The selection of adequate LC columns is required for the development of an optimal quantitative LC-MS/MS method. 20 In the present study, we implemented a dual-column LC-MS/MS. The serial combination of two different columns is known to be more effective in view of separating drugs and metabolites in complex matrices compared with single column methods.…”

Section: Discussionmentioning

confidence: 99%

Implementation of a Dual-Column Liquid Chromatography-Tandem Mass-Spectrometry Method for the Quantification of Isavuconazole in Clinical Practice

et al. 2021

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Objectives Therapeutic drug monitoring (TDM) of isavuconazole, which is a novel broad-spectrum antimycoticum against invasive fungal infections, ensures an effective exposure of the drug and minimizes the risk of toxicity. This study is aimed at evaluating the analytical performance of a dual-column liquid chromatography-tandem mass-spectrometry (LC-MS/MS) method for isavuconazole quantification. Materials and Methods The method was performed on a Voyager TSQ Quantum triple quadrupole instrument equipped with an Ultimate 3000 chromatography system (Thermo Fisher Scientific, San Jose, California, United States). Analytical and preanalytical requirements of the isavuconazole LC-MS/MS method were evaluated. Sample stability measurements were performed at room temperature (RT) and in serum tubes with separator gel. Results The isavuconazole LC-MS/MS method was linear over the concentration range of 0.2 to 12.8 mg/L. The coefficient of determination (r 2) always exceeded 0.999. Within- and between-run precision ranged between 1.4 to 2.9% and 1.5 to 3.0%, the recovery between 93.9 and 102.7%. At RT, serum samples were stable for 3 days. Isavuconazole serum concentrations were significantly lower after incubation (18 hours) in serum tubes with separator gel at RT. Conclusion The dual-column isavuconazole LC-MS/MS is a reliable tool for the TDM of isavuconazole. Serum samples are stable for at least 3 days and should be collected in tubes without separator gel.

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Section: Discussionmentioning

confidence: 99%

Implementation of a Dual-Column Liquid Chromatography-Tandem Mass-Spectrometry Method for the Quantification of Isavuconazole in Clinical Practice

et al. 2021

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“…First of all, method development scientists should not focus only on the use of acidic or neural mobile phases. The optimal buffer, ionization technique, ionization polarity and LC column cannot always be predicated from the compound properties, such as structure and p K a (Sillén & Magnell, ). The in‐silico predications or evaluations, albeit useful and broadly valid, cannot replace practical evaluation, especially when absolute sensitivity is paramount (Silvester, ).…”

Section: Futurementioning

confidence: 99%

Use of high‐pH (basic/alkaline) mobile phases for LC–MS or LC–MS/MS bioanalysis

Tan

Fanaras

2018

Biomedical Chromatography

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High-pH or basic/alkaline mobile phases are not commonly used in LC-MS or LC-MS/MS bioanalysis because of the deeply rooted concern with column instability and reduced detection sensitivity for basic compounds in high-pH mobile phases owing to charge neutralization. With the advancement of LC column technology and the wide recognition of the "wrong-way-round" phenomena, high-pH mobile phases are more and more used in LC-MS or LC-MS/MS bioanalysis to improve chromatographic peak shape, retention, selectivity, resolution, and detection sensitivity, not only for basic compounds, but also for many other compounds. In this article, the benefits, practical considerations, application examples and cautions for using high-pH mobile phases in LC-MS or LC-MS/MS bioanalysis are reviewed, with a focus on quantification. Furthermore, the future trends in this field are also envisaged.A total of 84 references are cited in this review. KEYWORDS alkaline mobile phase, basic mobile phase, bioanalysis, high pH, LC-MS, LC-MS/MS

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“…Two useful papers discuss remedies. 22,23 A strategy for column replacement needs to be established based on usage in relation to the cleanliness of sample extracts.…”

Section: Liquid Chromatographymentioning

confidence: 99%

Development and validation of a quantitative assay based on tandem mass spectrometry

Honour

2011

Ann Clin Biochem

115

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Many routine hospital and clinical research assays have relied upon immunoassay procedures to achieve sensitive measurements of a range of important analytes. Some of the methods have been developed in-house but increasingly commercial kits and automated analysers have become commonplace. The accuracies of these methods are under question in health care. Mass spectrometry (MS) is potentially a more accurate technique with the ability to demonstrate specificity. An introduction of the basic analytical aspects of liquid chromatography (LC) -MS/MS leads on to the validation of the method before general use. LC coupled with MS and tandem mass spectrometry (MS n ) is being adopted in a number of hospital laboratories for the quantitative analysis of a number of analytes from physiological matrices, but standards for development and validation of such assays are not easily available. Most assays can be regarded as in-house methods and herein may lay the failure so far for mass spectrometric methods to improve quality of results between laboratories for an analyte using the same technology. Manufacturers are taking on board the experience of clinical laboratories with kits containing all or most of the disposable items and reagents. A number of documents and guidelines have been consulted. These documents are expensive to purchase, are often very long and not easy to read. This review highlights the specific requirements for introduction of a tandem mass spectrometric test for small molecules into a routine hospital laboratory. A number of experiments need to be planned and executed in order to describe a new quantitative method in terms of selectivity, accuracy, imprecision, sensitivity and stability. The introduction of a quantitative method based on tandem MS requires careful validation. This review has distilled out important points from a number of key documents in order to provide a working validation guideline for clinical laboratories. In a supplementary file a working document for assembling the assay validation is proposed.

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Screening ionisation and chromatography conditions for quantitative LC/MS methods

Cited by 8 publications

References 26 publications

Implementation of a Dual-Column Liquid Chromatography-Tandem Mass-Spectrometry Method for the Quantification of Isavuconazole in Clinical Practice

Implementation of a Dual-Column Liquid Chromatography-Tandem Mass-Spectrometry Method for the Quantification of Isavuconazole in Clinical Practice

Use of high‐pH (basic/alkaline) mobile phases for LC–MS or LC–MS/MS bioanalysis

Development and validation of a quantitative assay based on tandem mass spectrometry

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