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Development of MEPS-UHPLC-MS/MS multistatin methods for clinical analysis
Hana Vlčková1, Pavel Svoboda1, Ondřej Novák2
1Department of Analytical Chemistry, Faculty of Pharmacy, Charles University, Heyrovského 1203, 500 05 Hradec Králové, Czech Republic.
Background:
Statins are the microsomal 3-hydroxy-3methylglutaryl-coenzyme A reductase inhibitors used for the treatment of hypercholesterolemia. Some recent studies revealed also the extra-lipid effects and anticancer activities. Due to the wide incidence of cancer diseases, the number of studies dealing with anticancer statin activities has grown in recent years. Development of one universal multistatin method will be a very convenient way of providing practical and economical multiple statin analysis. Results/methodology: Fast and sensitive methods for determination of seven clinically relevant statins, their interconversion products and metabolites (17 analytes in total) in biological samples using microextraction by packed sorbent for sample preparation and UHPLC-MS/MS for subsequent analysis were developed and validated. Three MS platforms with different ion sources, transfer optics, collision cell technologies and scan speed parameters were compared.
Conclusion:
Significant differences among the methods were observed in terms of selectivity and sensitivity. Microextraction by packed sorbent was successful in the extraction of all 17 analytes from biological matrix.
Insights
A new method efficiently analyzes seven statins and their metabolites in biological samples. This advancement offers a practical approach for studying statins' potential anticancer effects.
Area of Science:
- Pharmacology
- Analytical Chemistry
- Biochemistry
Background:
- Statins, HMG-CoA reductase inhibitors, are primarily used for hypercholesterolemia.
- Emerging research highlights statins' extra-lipid effects, including anticancer activities.
- The increasing incidence of cancer drives interest in statins' therapeutic potential.
Purpose of the Study:
- To develop a universal, sensitive, and practical method for analyzing multiple statins.
- To quantify seven clinically relevant statins and their metabolites in biological samples.
- To compare different mass spectrometry (MS) platforms for statin analysis.
Main Methods:
- Development and validation of a method using microextraction by packed sorbent (MEPS) for sample preparation.
- Utilized ultra-high-performance liquid chromatography coupled with tandem mass spectrometry (UHPLC-MS/MS) for analysis.
- Compared three distinct MS platforms regarding ion sources, optics, collision cell technology, and scan speed.
Main Results:
- Successfully developed and validated a method for determining 17 analytes (seven statins, interconversion products, and metabolites).
- Microextraction by packed sorbent proved effective for extracting all target analytes from biological matrices.
- Significant variations in selectivity and sensitivity were observed across the evaluated MS platforms.
Conclusions:
- The developed MEPS-UHPLC-MS/MS method is suitable for comprehensive statin analysis.
- The method's efficiency supports further research into statins' anticancer properties.
- Method optimization is crucial, as MS platform choice impacts analytical performance.
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