Systematic and comprehensive strategy for reducing matrix effects in LC/MS/MS analyses

doi:10.1016/J.JCHROMB.2006.12.030

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Systematic and comprehensive strategy for reducing matrix effects in LC/MS/MS analyses

Journal Article•DOI•

Systematic and comprehensive strategy for reducing matrix effects in LC/MS/MS analyses

Erin E. Chambers¹, Diane M. Wagrowski-Diehl¹, Ziling Lu¹, Jeffrey R. Mazzeo¹•Institutions (1)

Waters Corporation¹

01 Jun 2007-Journal of Chromatography B (Elsevier)-Vol. 852, Iss: 1, pp 22-34

TL;DR: The combination of polymeric mixed-mode SPE, the appropriate mobile phase pH and UPLC technology provides significant advantages for reducing matrix effects resulting from plasma matrix components and in improving the ruggedness and sensitivity of bioanalytical methods.

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About: This article is published in Journal of Chromatography B.The article was published on 2007-06-01. It has received 680 citations till now. The article focuses on the topics: Matrix (chemical analysis) & Sample preparation.

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Journal Article•DOI•

Validation of bioanalytical LC-MS/MS assays: evaluation of matrix effects.

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Ann Van Eeckhaut¹, Katrien Lanckmans¹, Sophie Sarre¹, Ilse Julia Smolders¹, Yvette Michotte¹ - Show less +1 more•Institutions (1)

Vrije Universiteit Brussel¹

01 Aug 2009-Journal of Chromatography B

TL;DR: In this review, the influence of matrix effects on bioanalytical LC-MS/MS methods is discussed and illustrated with some examples, and possible solutions to reduce or eliminate matrix effects are highlighted.

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692 citations

Journal Article•DOI•

An overview of matrix effects in liquid chromatography-mass spectrometry.

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Helga Trufelli¹, Pierangela Palma¹, Giorgio Famiglini¹, Achille Cappiello¹•Institutions (1)

University of Urbino¹

01 May 2011-Mass Spectrometry Reviews

TL;DR: This review gives a detailed description on when matrix effects (ME) might be expected, and how they can be evaluated, and the main strategies to overcome these phenomena are described in detail.

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Abstract: Matrix-dependent signal suppression or enhancement represents a major drawback in quantitative analysis with liquid chromatography coupled to atmospheric pressure ionization mass spectrometry (LC-API-MS). Because matrix effects (ME) might exert a detrimental impact on important method parameters (limit of detection, limit of quantification, linearity, accuracy, and precision), they have to be tested and evaluated during validation procedure. This review gives a detailed description on when these phenomena might be expected, and how they can be evaluated. The major sources of ME are discussed and illustrated with examples from bioanalytical, pharmaceutical, environmental, and food analysis. Because there is no universal solution for ME, the main strategies to overcome these phenomena are described in detail. Special emphasis is devoted to the sample-preparation procedures as well as to the recent improvements on chromatographic and mass spectrometric conditions. An overview of the main calibration techniques to compensate for ME is also presented. All these solutions can be used alone or in combination to retrieve the performance of the LC-MS for a particular matrix-analyte combination.

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631 citations

Cites background or methods or result from "Systematic and comprehensive strate..."

...…front, where highly polar and unretained compounds are eluted, and the end of the elution gradient, where the strongly retained compounds are eluted (Bonfiglio et al., 1999; van Hout et al., 2000; Müller et al., 2002; Shou & Weng, 2003; Souverain, Rudaz, & Veuthey, 2004; Chambers et al., 2007)....
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...With the post-extraction addition method, Chambers and co-workers evaluated several clean-up methods to detect basic and neutral drugs in rat plasma samples, including PPT, LLE, and SPE with respect to ME and recovery (Chambers et al., 2007)....
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...The improved resolution provides a benefit with respect to ME, through improved separation from endogenous components (Chambers et al., 2007; Marı́n et al., 2009)....
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...Usually the chromatographic areas that aremost affected by interferences are the solvent front, where highly polar and unretained compounds are eluted, and the end of the elution gradient, where the strongly retained compounds are eluted (Bonfiglio et al., 1999; van Hout et al., 2000; Müller et al., 2002; Shou & Weng, 2003; Souverain, Rudaz, & Veuthey, 2004; Chambers et al., 2007)....
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...Recently, mixed-mode SPE has been proposed as an effective tool to reduceME (Müller et al., 2002;Mallet, Lu, &Mazzeo, 2004; Chambers et al., 2007)....
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Journal Article•DOI•

Overcoming matrix effects using the dilution approach in multiresidue methods for fruits and vegetables.

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Carmen María Salvador Ferrer¹, Ana Lozano¹, Ana Agüera¹, A. Jiménez Girón¹, Amadeo R. Fernández-Alba¹ - Show less +1 more•Institutions (1)

University of Almería¹

21 Oct 2011-Journal of Chromatography A

TL;DR: In this work, matrix effects of 53 pesticides in three different matrices were evaluated and a dilution factor of 15 demonstrated to be enough to eliminate most of the matrix effects, opening the possibility to perform quantification with solvent based standards in the majority of the cases.

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350 citations

Journal Article•DOI•

Tutorial review on validation of liquid chromatography-mass spectrometry methods: part II.

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Anneli Kruve¹, Riin Rebane¹, Karin Kipper¹, Maarja-Liisa Oldekop¹, Hanno Evard¹, Koit Herodes¹, Pekka Ravio, Ivo Leito¹ - Show less +4 more•Institutions (1)

University of Tartu¹

22 Apr 2015-Analytica Chimica Acta

TL;DR: This is the part II of a tutorial review intending to give an overview of the state of the art of method validation in liquid chromatography mass spectrometry and discuss specific issues that arise with MS (and MS-MS) detection in LC (as opposed to the "conventional" detectors).

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249 citations

Journal Article•DOI•

Biological Matrix Effects in Quantitative Tandem Mass Spectrometry-Based Analytical Methods: Advancing Biomonitoring

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Parinya Panuwet¹, Ronald E. Hunter², Priya E. D’Souza¹, Xianyu Chen¹, Samantha A. Radford¹, Jordan R. Cohen¹, M. Elizabeth Marder¹, Kostya Kartavenka¹, P. Barry Ryan¹, Dana B. Barr¹ - Show less +6 more•Institutions (2)

Emory University¹, Centers for Disease Control and Prevention²

03 Mar 2016-Critical Reviews in Analytical Chemistry

TL;DR: The ability to quantify levels of target analytes in biological samples accurately and precisely in biomonitoring involves the use of highly sensitive and selective instrumentation such as tandem mass spectrometers and a thorough understanding of highly variable matrix effects.

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Abstract: The ability to quantify levels of target analytes in biological samples accurately and precisely in biomonitoring involves the use of highly sensitive and selective instrumentation such as tandem mass spectrometers and a thorough understanding of highly variable matrix effects. Typically, matrix effects are caused by co-eluting matrix components that alter the ionization of target analytes as well as the chromatographic response of target analytes, leading to reduced or increased sensitivity of the analysis. Thus, before the desired accuracy and precision standards of laboratory data are achieved, these effects must be characterized and controlled. Here we present our review and observations of matrix effects encountered during the validation and implementation of tandem mass spectrometry-based analytical methods. We also provide systematic, comprehensive laboratory strategies needed to control challenges posed by matrix effects in order to ensure delivery of the most accurate data for biomonitoring studies assessing exposure to environmental toxicants.

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230 citations

Cites background or methods or result from "Systematic and comprehensive strate..."

...Chambers et al. (2007) stated that mixed-mode reversed-phase/ion exchange cartridges generally provide cleaner samples and therefore reduced ion suppression in LC-MS/MS systems, but our results suggest otherwise....
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...© 2016 Taylor and Francis Group, LLC either high performance (HP)-LC or GC-MS methods (Chambers et al., 2007; Mei et al., 2003)....
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...It is important that matrix effects be investigated and managed during the validation and implementation of a method because they can lead to inaccurate measurements of target compounds (Chambers et al., 2007; Chiu et al., 2010; Hajslova and Zrostlikova, 2003)....
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...either high performance (HP)-LC or GC-MS methods (Chambers et al., 2007; Mei et al., 2003)....
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References

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Journal Article•DOI•

Strategies for the assessment of matrix effect in quantitative bioanalytical methods based on HPLC-MS/MS.

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Bogdan K. Matuszewski¹, M.L Constanzer¹, C.M Chavez-Eng¹•Institutions (1)

United States Military Academy¹

04 Jun 2003-Analytical Chemistry

TL;DR: Practical, experimental approaches for studying, identifying, and eliminating the effect of matrix on the results of quantitative analyses by HPLC-MS/MS are described and it is demonstrated that, for the investigational drug under study, the matrix effect was clearly observed when ISP interface was utilized but it was absent when the HN interface was employed.

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Abstract: In recent years, high-performance liquid chromatography (HPLC) with tandem mass spectrometric (MS/MS) detection has been demonstrated to be a powerful technique for the quantitative determination of drugs and metabolites in biological fluids. However, the common and early perception that utilization of HPLC−MS/MS practically guarantees selectivity is being challenged by a number of reported examples of lack of selectivity due to ion suppression or enhancement caused by the sample matrix and interferences from metabolites. In light of these serious method liabilities, questions about how to develop and validate reliable HPLC−MS/MS methods, especially for supporting long-term human pharmacokinetic studies, are being raised. The central issue is what experiments, in addition to the validation data usually provided for the conventional bioanalytical methods, need to be conducted to confirm HPLC−MS/MS assay selectivity and reliability. The current regulatory requirements include the need for the assessment and...

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4,543 citations

Journal Article•DOI•

Matrix effects: the Achilles heel of quantitative high-performance liquid chromatography-electrospray-tandem mass spectrometry.

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Paul J. Taylor¹•Institutions (1)

Princess Alexandra Hospital¹

01 Apr 2005-Clinical Biochemistry

TL;DR: The major aspects of matrix effects are discussed with an approach to address matrix effects during method validation proposed.

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1,127 citations

Journal Article•DOI•

Mechanistic investigation of ionization suppression in electrospray ionization.

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Richard King¹, Ryan Bonfiglio¹, Carmen Fernandez-Metzler¹, Cynthia Miller-Stein¹, Timothy V. Olah¹ - Show less +1 more•Institutions (1)

United States Military Academy¹

01 Nov 2000-Journal of the American Society for Mass Spectrometry

TL;DR: Results point to changes in the droplet solution properties caused by the presence of nonvolatile solutes as the main cause of ionization suppression in electrospray ionization of biological extracts.

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1,012 citations

Journal Article•DOI•

Matrix effect in quantitative LC/MS/MS analyses of biological fluids: a method for determination of finasteride in human plasma at picogram per milliliter concentrations.

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Bogdan K. Matuszewski¹, M.L. Constanzer, C.M Chavez-Eng•Institutions (1)

United States Military Academy¹

04 Feb 1998-Analytical Chemistry

TL;DR: Development of a highly sensitive assay for I in human plasma at low picogram per milliliter concentrations using LC/MS/MS with a heated nebulizer (HN) interface, instead of a TISP interface, is described, practically eliminating the ion suppression.

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Abstract: Contrary to common perceptions, the reliability of quantitative assays for the determination of drugs in biological fluids using high-performance liquid chromatography with tandem mass spectrometric (LC/MS/MS) detection methods and the integrity of resulting pharmacokinetic data may not be absolute. Results may be adversely affected by lack of specificity and selectivity due to ion suppression caused by the sample matrix, interferences from metabolites, and “cross-talk” effects. In this paper, an example of the effect of the sample matrix on the determination of finasteride (I) in human plasma is presented. The ion suppression effect was studied by analyzing standards of I injected directly in mobile phase and comparing the response (peak areas) of I and an internal standard (II) with the peak areas of the same analytes spiked before extraction into five different plasma pools and standards spiked into the plasma extracts after extraction. The LC/MS/MS analyses were performed using a turbo ion spray inter...

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876 citations

Journal Article•DOI•

From ions in solution to ions in the gas phase - the mechanism of electrospray mass spectrometry

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Paul Kebarle, Liang. Tang

15 Nov 1993-Analytical Chemistry

736 citations