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To estimate the recovery of each analyte from the extraction, the response ratio of each analyte over the respective internal standard was used, and to estimate matrix effects, the absolute response (peak area) of each analyte was used.
In order to avoid the generation of biased data due to matrix effects, the developed LC-MS/MS method had to be properly validated.
Taking into consideration that XRF suffers from matrix effects, the agreement between the two methods was satisfactory; the difference was statistically not significant (p = 0.1).
To compensate for the lack of isotope-labeled internal standards for the other analytes and to partially account for matrix effects, the calibration standards were spiked into calf serum.
While isotope dilution mass spectrometry is capable to deliver unbiased results even in the presence of severe matrix effects, the control of these effects through appropriate measures will improve accuracy.
To prevent excessive matrix effects, the analytes were separated from the matrix constituents using a column-switch liquid chromatography system combining a reversed-phase and a Hypercarb analytical column.
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In order to alleviate this matrix effect, the standard addition calibration method was used for quantitative determination.
Despite a small sample matrix effect, the sensitivity of the assay falls well into EU regulatory limits.
Again, from the obtained recovery percentage (85.4 107% w/w), the matrix effects of the samples were not considerable.
Based on the obtained recovery percentage, 85.4 107% (w/w), the matrix effects of the samples were not considerable.
The matrix effects on the extracted samples were significantly observed in low concentration (10 ng/ml) samples (Fig. 1).
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