摘要
This paper describes the optimisation and validation of an ultra performance liquid chromatography- tandem mass spectrometry (UPLC-MS/MS) method for the analysis of four pharmaceuticals (flubendazole, pipamperone, rabeprazole and domperidone) and one pesticide (propiconazole) in surface water. Sample preparation was reduced substantially as compared to a previously published high performance liquid chromatography-tandem mass spectrometry (LC-MS/MS) method, thanks to the use of UPLC. In addition, internal standards could now be used for quantification instead of the standard addition method. Extraction was performed on a Speedisk phenyl solid-phase extraction tube. A Waters Acquity HSS T3 UPLC column (100 x 2.1mm i.d.; 1.8-mu m particles) was used for separation and an API 4000 triple quadrupole was used as a detector. Total run time was 8.59 minutes. Matrix effects were examined on different surface water samples. Limits of detection and quantification in surface water samples were between 100 and 500 pg/l. Validation was performed on surface water. The method showed good precision (<15%) and accuracy (85-120%). This method is less time-consuming and labour-intensive than a previously published HPLC-procedure without compromising validation parameters.
- 出版日期2011