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A multidrug LC-MS/MS method for the determination of five immunosuppressants in oral fluid

机译：多药LC-MS / MS方法，用于测定口腔液中五种免疫抑制剂

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Aim: This study aimed: to develop and validate an LC-MS/MS method for mycophenolic acid, tacrolimus, sirolimus, everolimus and cyclosporin A in oral fluid (OF), as an essential tool to study the usefulness of OF as an alternative matrix for immunossuppressants' therapeutic drug monitoring; and to find the best OF collector for these analytes. Materials & Methods: Chromatographic separation was achieved using an XBridge R Shield RP18 analytical column maintained at 65oC, using 2 mM ammonium formate and 0.1% formic acid in water (A) and acetonitrile (B) as mobile phase. OF sample was extracted with solid phase extraction after sonication and protein precipitation. Results & Conclusions: Method validation met all the acceptance criteria. LODs were 0.05-1 ng/ml, and LOQs 0.1-5 ng/ml. Silanized tubes offered the best recoveries. The method was successfully applied to 31 OF specimens, describing everolimus detection in OF for the first time. Conclusion: The proposed method is sensitive enough for the detection of OF trough concentrations in patients receiving immunosuppressants when using an appropriate OF collector.
机译：目的：本研究旨在开发和验证用于霉酚酸，躯干司，西罗莫司，血吸虫和口服液（OF）中的环孢菌素A的LC-MS / MS方法，作为研究作为作为替代基质的有用性的必要工具用于免疫抑制剂的治疗药物监测;并找到这些分析物中最好的收集器。材料和方法：使用在65oC的Xbridge R屏蔽RP18分析柱实现色谱分离，使用2mM甲酸铵和0.1％甲酸在水（A）和乙腈（B）中作为流动相。在超声处理和蛋白质沉淀后用固相提取萃取样品。结果与结论：方法验证符合所有验收标准。 LOD为0.05-1ng / ml，LOQs 0.1-5 ng / ml。硅烷化管提供了最好的回收率。该方法成功地应用于31种标本，首次描述了血尿症率检测。结论：当使用收集器的适当时，所提出的方法足以检测接受免疫抑制剂的患者患者的槽浓度。

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