Determination of Prazosin and Simvastatin in Landfill Leachate Using Liquid Chromatography-Time of Flight-Mass Spectrometry

Abstract

Human pharmaceuticals have been shown to occur in considerably high amounts in sewage treatment plant (STP) effluents and surface waters. So far there is no data available on the occurrence of prazosin and simvastatin in leachate sample in Malaysia. Thus, this study is the first report to analysis of prazosin and simvastatin in leachate samples by using solid phase extractionliquid chromatography-time of flight-mass spectrometry (SPE-LC-TOF-MS). The proposed method included isolation and reconstitute procedure. The linearity range was achieved at 1.5 -3000 μg/L and 0.8 -125 μg/L for prazosin and simvstatin, respectively with a determination coefficient (R 2 ) > 0.99. The limit of quantification (LOQ) for prazosin and simvastatin was calculated at 2.1 and 0.5 ng/L in deionised water (DIW), meanwhile it was recorded at 3.5 and 2.4 ng/L for prazosin and simvastatin in effluent sample, respectively. Two pharmaceutical compounds were detected in the leachate samples: prazosin and simvastatin at concentrations levels of 3850 and 415 ng/L, respectively.Keywords: prazosin, simvastatin, leachate, solid phase extraction, pharmaceutical pollution Abstrak Farmaseutikal manusia telah hadir di dalam effluen loji sisa rawatan dan air permukaan. Sehingga kini, tiada data kajian yang merekodkan kehadiran prazosin dan simvastatin dalam sampel larut lesap di Malaysia. Maka, kajian ini merupakan laporan pertama tentang analisis terhadap prazosin dan simvastatin di dalam sampel larut lesap mengunakan pengekstrakan fasa pepejalkromatografi cecair-masa penerbangan-spekrometri jisim (SPE-LC-TOF-MS). Kaedah yang dibangun meliputi langkah pemisahan dan nilai isian semula. Julat kelinearan dicapai antara 1.5 -3000 μg/L dan 0.8 -125 μg/L masing -masing bagi prazosin dan simvastatin dengan nilai pekali (R 2 ) > 0.99. Had kuantifikasi (LOQ) bagi prazosin and simvastatin dihitung pada aras 2.1 dan 0.5 ng/L di dalam air ternyahion manakala direkod masing-masing pada aras 3.5 dan 2.4 ng/L di dalam sampel efluen. Dua jenis sebatian farmaseutikal ini dikesan in dalam sampel larut lesap pada aras kepekatan masing-masing adalah 3850 and 415 ng/L. Kata kunci: prazosin, simvastatin, larut lesap, pengekstrakan fasa pepejal, pencemaran farmaseutikal