کد مقاله کد نشریه سال انتشار مقاله انگلیسی نسخه تمام متن
1202183 965060 2011 8 صفحه PDF دانلود رایگان
عنوان انگلیسی مقاله ISI
Automated method for targeting analysis of prostanoids in human serum by on-line solid-phase extraction and liquid chromatography–mass spectrometry in selected reaction monitoring
موضوعات مرتبط
مهندسی و علوم پایه شیمی شیمی آنالیزی یا شیمی تجزیه
پیش نمایش صفحه اول مقاله
Automated method for targeting analysis of prostanoids in human serum by on-line solid-phase extraction and liquid chromatography–mass spectrometry in selected reaction monitoring
چکیده انگلیسی

Prostanoids are potent biologically active lipid molecules demanding for analysis methods combining precision, sensitivity and high-throughput for pharmacological and clinical applications. The present research describes the development and validation of an on-line automated method based on solid-phase extraction liquid chromatography–tandem mass spectrometry (SPE–LC–MS/MS) for the quantification of prostanoids in human serum. This approach overcomes the main limitation of previous methods involving manual protocols, such as analyte losses, metabolites degradation and time-consuming protocols, are minimized. Human serum (100 μL) was directly injected into an automatic solid-phase extraction workstation for cleanup and preconcentration of the target metabolites. The eluate was on-line transferred to a reversed-phase analytical column for chromatographic separation prior to mass spectrometry detection in selected reaction monitoring mode. The detection limits for the target analytes ranged from 2.3 to 63.3 pg on column. The precision (expressed as relative standard deviation) was within 3.30 and 6.15% for repeatability and from 4.16 to 11.11% for within-laboratory reproducibility. Accuracy was evaluated with spiked and non-spiked serum samples to estimate concentration differences that could be affected by matrix effects or inefficient SPE performance. Accuracy, estimated as recovery factor, was from 87.7 to 100% for the target compounds. The proposed method is reliable and has an excellent potential for high-throughput use in both clinical and research laboratories by minimizing analyst intervention.

ناشر
Database: Elsevier - ScienceDirect (ساینس دایرکت)
Journal: Journal of Chromatography A - Volume 1218, Issue 20, 20 May 2011, Pages 2848–2855
نویسندگان
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