A liquid chromatography-tandem mass spectrometry method for the determination of nodularin-R in human plasma and its preliminary clinical application

作者：Yu, Ying; Xu, Jinhui; Liu, Yuan; Qiao, Shanlei; Chen, Yun^*

来源：Clinica Chimica Acta, 2012, 413(9-10): 894-900.

DOI：10.1016/j.cca.2012.01.039

• Nodularin-R
• Liquid chromatography-tandem mass spectrometry
• Method validation
• Human plasma
• Immunoassay
• Demographic factors

Background: Nodularins are an important class of hepatotoxic cyclic pentapeptides that most current methods are ill-suited to clinically monitor. Therefore, a liquid chromatography-tandem mass spectrometry (LC/MS/MS) assay for the determination of nodularin-R in human plasma was validated and applied to clinical samples in this report. @@@ Methods: Sample cleanup and enrichment were achieved using solid phase extraction. The concentration of nodularin-R in each sample was calculated using the relative abundance area ratio of nodularin-R and a stable isotope-labeled internal standard. @@@ Results: The validated calibration range was from 0.50 to 100 ng/ml. The intra- and inter-day precision were <6.0 and 9.8%, respectively. The accuracy at the lower limit of quantification (LLOQ) was 2.0%, while for other QC levels, it was <3.4%. The absolute concentrations determined by the LC/MS/MS assay were significantly lower than those measured using a commercial immunoassay. Finally, a variety of demographic factors were evaluated and the findings indicated that the elderly (>50 y) and people living close to seashore or lakefront areas (<= 10 km) were the most susceptible to nodularin-R (p = 0.79 x 10(-4) and 2.57 x 10(-6), respectively). @@@ Conclusions: This report was among the first to demonstrate that clinical monitoring of nodularin-R could be achieved using LC/MS/MS.

• 出版日期2012-5-18
• 单位南京医科大学