Center for Advanced Water Technology, PUB, the Toh Tuck Complex, 82, Toh Guan Road East, Singapore 608575, Singapore.
J Chromatogr A. 2010 Feb 26;1217(9):1471-5. doi: 10.1016/j.chroma.2009.12.074. Epub 2010 Jan 4.
Matrix effect is a major problem when trace level pharmaceuticals in seawater were analyzed using solid-phase extraction (SPE) combined with high-performance liquid chromatography-electrospray ionization tandem mass spectrometry (HPLC-ESI-MS-MS). Therefore, efforts should be devoted to diminish matrix effect as much as possible. The present study investigates the matrix effect during the analysis of selected pharmaceutical residues (naproxen, ibuprofen, diclofenac and gemfibrozil) in seawater samples with ultra-high-performance liquid chromatography (UHPLC)-ESI low-energy collision-induced dissociation (CID) MS-MS. Solutions to reduce matrix effect were studied through optimization of SPE procedure and the employment of isotope-labeled analogues. Results showed that 30 mL of deionized water can efficiently diminish matrix effect and satisfactory absolute mean recoveries ranging from 73.5% to 120.5% were obtained in the optimized SPE condition. Isotope-labeled analogues employed as surrogates were found to be efficient to further compensate for matrix effect, with the relative mean recoveries ranging from 85.5% to 110.5%. The optimized method has been successfully applied for the analysis of target pharmaceutical residues in different seawater samples.
当使用固相萃取（SPE）结合高效液相色谱-电喷雾串联质谱（HPLC-ESI-MS-MS）分析海水中痕量药物时，基质效应是一个主要问题。因此，应努力尽可能减少基质效应。本研究采用超高效液相色谱（UHPLC）-电喷雾低能碰撞诱导解离（CID）MS-MS 研究了海水样品中选定药物残留（萘普生、布洛芬、双氯芬酸和吉非贝齐）分析过程中的基质效应。通过优化 SPE 程序和使用同位素标记类似物来研究减少基质效应的方法。结果表明，30 mL 去离子水可有效减少基质效应，在优化的 SPE 条件下，获得了令人满意的绝对平均回收率范围为 73.5%至 120.5%。作为替代品使用的同位素标记类似物被发现可有效进一步补偿基质效应，相对平均回收率范围为 85.5%至 110.5%。优化后的方法已成功应用于不同海水样品中目标药物残留的分析。
