Abstract：
:Ultratrace analysis of sample components requires excellent analytical performance in terms of limits of quantitation (LoQ). Micro UHPLC coupling with sensitive tandem mass spectrometry provides state of the art solutions for such analytical problems. Decreased column volume in micro LC limits the injectable sample volume. However, if analyte concentration is extremely low, it might be necessary to inject high sample volumes. This is particularly critical for strong sample solvents and weakly retained analytes, which are often the case when preparing biological samples (protein precipitation, sample extraction, etc.). In that case, high injection volumes may cause band broadening, peak distortion or even elution in dead volume. In this study, we evaluated possibilities of high volume injection onto microbore RP-LC columns, when sample solvent is diluted. The presented micro RP-LC-MS/MS method was optimized for the analysis of steroid hormones from human plasma after protein precipitation with organic solvents. A proper sample dilution procedure helps to increase the injection volume without compromising peak shapes. Finally, due to increased injection volume, the limit of quantitation can be decreased by a factor of 2-5, depending on the analytes and the experimental conditions.
journal_name
J Pharm Biomed Analjournal_title
Journal of pharmaceutical and biomedical analysisauthors
Márta Z,Bobály B,Fekete J,Magda B,Imre T,Mészáros KV,Szabó PTdoi
10.1016/j.jpba.2016.06.024subject
Has Abstractpub_date
2016-09-10 00:00:00pages
135-141eissn
0731-7085issn
1873-264Xpii
S0731-7085(16)30341-7journal_volume
129pub_type
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journal_title：Journal of pharmaceutical and biomedical analysis
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journal_title：Journal of pharmaceutical and biomedical analysis
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journal_title：Journal of pharmaceutical and biomedical analysis
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doi：10.1016/j.jpba.2017.02.027
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