Liquid chromatography matrix effects

Table 5.15 Relative signal responses from various injection volumes for the LC-MS-MS analysis of a wheat forage matrix sample. Reprinted from J. Chromatogr., A, 907, Choi, B. K., Hercules, D. M. and Gusev, A. L, Effect of liquid chromatography separation of complex matrices on liquid chromatography-tandem mass spectrometry signal suppression , 337-342, Copyright (2001), with permission from Elsevier Science...

The method for chloroacetanilide soil metabolites in water determines concentrations of ethanesulfonic acid (ESA) and oxanilic acid (OXA) metabolites of alachlor, acetochlor, and metolachlor in surface water and groundwater samples by direct aqueous injection LC/MS/MS. After injection, compounds are separated by reversed-phase HPLC and introduced into the mass spectrometer with a TurboIonSpray atmospheric pressure ionization (API) interface. Using direct aqueous injection without prior SPE and/or concentration minimizes losses and greatly simplifies the analytical procedure. Standard addition experiments can be used to check for matrix effects. With multiple-reaction monitoring in the negative electrospray ionization mode, LC/MS/MS provides superior specificity and sensitivity compared with conventional liquid chromatography/mass spectrometry (LC/MS) or liquid chromatography/ultraviolet detection (LC/UV), and the need for a confirmatory method is eliminated. In summary,... 

Using a simple solvent extraction procedure to minimize matrix effects, a diclofop-methyl immunoassay was developed for milk, a number of edible plant products, and other matrices. Gas chromatography (GC) and liquid scintillation counting (LSC) of a C-labeled analyte were used as reference methods to compare with enzyme immunoassay (EIA) results. The methods were well correlated, with comparison of EIA... 

Hsieh Y. et al., 2001. Quantitative screening and matrix effect studies of drug discovery compounds in monkey plasma using fast-gradient liquid chromatography/tandem mass spectrometry. Rapid Commun Mass Spectrom 15 2481. 

Hydrophilic interaction liquid chromatography (HILIC) can handle the matrix effects nonvolatiles, which may reduce the evaporation of volatile ions during the electrospray process. Ion-exchange methods that require the use of salts could otherwise interfere with MS. 

In standard FAB, the surface of the matrix solution is depleted of analyte and suffers from radiational damage during elongated measurements. Refreshment of the surface proceeds by diffusion (limited by the viscosity of the matrix) or evaporation. Continuous-flow fast atom bombardment (CF-FAB) continuously refreshes the surface exposed to the atom beam. [107,108] The same effect is obtained in slightly different way by the frit-fast atom bombardment (frit-FAB) technique. [109,110] In addition, both CF-FAB and frit-FAB can be used for online-coupling of liquid chromatography (LC, Chap. 12) [111] or capillary electrophoresis (CE) to a FAB ion source. [112]... 

Mei H, Hseih Y, Nardo C, Xu X, Wang S, et al. 2003. Investigation of matrix effects in bioanalytical high performance liquid chromatography/tandem, mass spectrometrometic assay application to drug discovery. Rapid Commun Mass Spectrom 17 97-103. 

Jemal, M., Schuster, A., and Whigan, D. B. (2003). Liquid chromatography/tandem mass spectrometry methods for quantitation of mevalonic acid in human plasma and urine method validation, demonstration of using a surrogate analyte, and demonstration of unacceptable matrix effect in spite of use of a stable isotope analog internal standard. Rapid Commun. Mass Spectrom. 17, 1723-1734. 

Tiller, P. R. Romanyshyn, L. A. Implications of matrix effects in ultrafast gradient or fast isocratic liquid chromatography with mass spectrometry in drug discovery. Rapid Commun Mass Spectrom 2002, 16, 92-98. 

Taylor, P. J. Matrix effects the Achilles heel of quantitative high-performance liquid chromatography-electrospray-tandem mass spectrometry. Clin Biochem 2005, 38, 328-334. 

Xu, X. Mei, H. Wang, S. Zhou, Q. Wang, G. et ah A study of common discovery dosing formulation components and their potential for causing time-dependent matrix effects in high-performance liquid chromatography tandem mass... 

Ylinen et al. [53] developed an ion-pair extraction procedure employing tetrabutylamonium (TBA) counter ions for determination of PFOA in plasma and urine in combination with gas chromatography (GC) and flame ionisation detection (FID). Later on, Hansen et al. [35] improved the sensitivity of the ion-pair extraction approach using methyl tertiary butyl ether (MTBE) and by the inclusion of a filtration step to remove solids from the extract making it amenable to liquid chromatography coupled to tandem mass spectrometry (LC-MS/MS) determination. Ion-pair extraction procedure has been the basis of several procedures for biota [49,54-58] and food samples [50,59,60]. However, this method has shown to have some limitations, such as (1) co-extraction of lipids and other matrix constituents and the absence of a clean-up step to overcome the effects of matrix compounds and (2) the wide variety of recoveries observed, typically ranging. 

Marin JM, Gracia-Lor E, Sancho JV et al (2009) Application of ultra-high-pressure liquid chromatography-tandem mass spectrometry to the determination of multi-class pesticides in environmental and wastewater samples Study of matrix effects. J Chromatogr A 1216 1410-1420... 

Hsieh, Y., Chintala, M., Mei, H., Agans, J., Brisson, J. M., Ng, K., and Korfmacher, W. A. (2001). Quantitative screening and matrix effect studies of drug discovery compounds in monkey plasma [by] using fast-gradient liquid chromatography/tandem mass spectrometry. Rapid Commun. Mass Spectrom. 15 2481-2487. 

Liquid chromatography (also called adsorption chromatography) has helped to characterize the group composition of crude oils and hydrocarbon products since the beginning of this century. The type and relative amount of certain hydrocarbon classes in the matrix can have a profound effect on the quality and performance of the hydrocarbon product. The fluorescent indicator adsorption (FIA) method (ASTM D-1319) has been used to measure the paraffinic, olefinic, and aromatic content of gasoline, jet fuel, and liquid products in general (Suatoni and Garber, 1975 Miller et al., 1983 Norris and Rawdon, 1984). 

A selective, sensitive, and rapid hydrophilic interaction liquid chromatography with electrospray ionization tandem mass spectrometry was developed for the determination of donepezil in human plasma [32], Donepezil was twice extracted from human plasma using methyl-ferf-butyl ether at basic pH. The analytes were separated on an Atlantis HILIC Silica column with the mobile phase of acetonitrile ammonium formate (50 mM, pH 4.0) (85 15, v/v) and detected by tandem mass spectrometry in the selective reaction monitoring mode. The calibration curve was linear (r = 0.9994) over the concentration range of 0.10-50.0 ng/ ml and the lower limit of quantification was 0.1 ng/ml using 200 /d plasma sample. The CV and relative error for intra- and inter-assay at four quality control levels were 2.7% to 10.5% and —10.0% to 0.0%, respectively. There was no matrix effect for donepezil and cisapride. The present method was successfully applied to the pharmacokinetic study of donepezil after oral dose of donepezil hydrochloride (10 mg tablet) to male healthy volunteers. 

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