Please use this identifier to cite or link to this item:
https://ptsldigital.ukm.my/jspui/handle/123456789/499710Full metadata record
| DC Field | Value | Language |
|---|---|---|
| dc.contributor.advisor | Md Pauzi Abdullah, Professor Dr. | - |
| dc.contributor.author | Al-Qaim Fouad Fadhil Mohamed Hussain (P55923) | - |
| dc.date.accessioned | 2023-10-13T09:33:58Z | - |
| dc.date.available | 2023-10-13T09:33:58Z | - |
| dc.date.issued | 2015-04-06 | - |
| dc.identifier.other | ukmvital:81691 | - |
| dc.identifier.uri | https://ptsldigital.ukm.my/jspui/handle/123456789/499710 | - |
| dc.description | The occurrence of pharmaceutical residue in the Malaysian aquatic environment effectively has never been reported. The main objective for this work is to develop a comprehensive method for analysis of 11 selected pharmaceutical residues in different matrices namely surface water, sewage treatment plants effluent and influent, and hospitals effluent and influent. The developed method involved the isolation and concentration with solid phase extraction (SPE) followed by a separation and detection using a highly sensitive and selective instrument i.e. liquid chromatographytime of flight/mass spectrometry (LC-TOF/MS). The SPE has been optimized in terms of type of sorbent, elution solvent and flow rate of loading sample to get good recoveries considering the different physicochemical properties in terms of pKa and logKow of the target compounds. To increase the selectivity of TOF measurements, a narrow accurate mass interval was used to reconstruct the chromatographic traces. Extracted ion chromatograms (EIC) were typically extracted using a 20 mDa mass window for all target compounds. However, reducing the mass window from 500 to 20 mDa resulted in an almost two-fourfold increase of the signal to noise (S/N) ratio. The method was validated for drinking water (DW), surface water (SW), sewage treatment plant (STP) influent and effluent, and hospital (HSP) influent and effluent. The Instrumental detection limits IDLs were (in μg/L) 5.0, 1.5, 0.8, 1.5, 0.8, 0.3, 5.0, 0.8, 3.0, 5.0 and 1.5 for caffeine, prazosin, enalapril, carbamazepine, nifedipine, gliclazide, levonorgestrel, simvastatin, hydrochlorothiazide, diclofenac-Na and mefenamic acid. The limits of quantification (LOQ) were as low as 0.4, 1.6, 5, 2.8, 2.2 and 11 ng/L in DW, SW, HSP influent and effluent, STP effluent and influent, respectively. In general, good recoveries of higher than 70% were obtained for most of the target analytes in all matrices. Matrix effect was evaluated for all samples matrices. The proposed method was successfully used to determine and quantify the target compounds in raw and treated wastewater of four sewage treatment plants and three hospitals in Malaysia, as well as in two receiving surface water sites. The results showed that a number of the studied compounds namely; caffeine, carbamazepine, gliclazide simvastatin, hydrochlorothiazide and mefenamic acid pose moderate to high persistency in sewage treatment effluents as well as in the receiving rivers. The frequency of detection for all compounds in all sampling points during nine months monitoring (from April to December 2013) involving 105 samples were as follow: caffeine 81% (85:105), prazosin 47% (49:105), enalpril 24% (25:105), carbamazepine 78% (82:105), gliclazide 92.7% (89:96), levonorgestrel 27.6% (29:105), simvastatin 40% (42:105), hydrochlorothiazide 81% (85:105), diclofenac-Na 32.4% (34:105) and mefenamic acid 56.2% (59:105). Nifedipine has been detected only two times out of 105 samples. The mean concentration of the detected pharmaceuticals in STP influent and effluent, hospital influent and effluent, and receiving surface water was ranged from ˂ LOQ to 3700 ng/L and 11 to 577 ng/L, 19 to 1419 ng/L and 19 to 1468 ng/L, and 5 to 427 ng/L, respectively. The highest concentration detected in sampling points was for caffeine 9099 ng/L. Multivariant analysis involving, cluster analysis, principal component analysis and factor analysis was used to assess the occurrence of pharmaceuticals in water samples. In the light of the results, prazosin and gliclazide were detected for the first time in aquatic environment. This study has confirmed that the Malaysian aquatic environment is impacted by various pharmaceutical residues at varying levels.,Kehadiran farmaseutikal di dalam persekitaran akuatik Malaysia belum pernah dilaporkan secara efektif. Objektif utama kajian ini adalah untuk membangunkan suatu kaedah analisis yang komprehensif terhadap 11 sisa farmaseutikal terpilih di dalam pelbagai matriks seperti air permukaan, influen dan efluen loji rawatan kumbahan dan hospital. Kaedah yang dibangunkan merangkumi pengasingan dan pemekatan melalui pengekstrakan fasa pepejal (SPE) diikuti dengan pemisahan dan pengesanan menggunakan alat yang sangat peka dan selektif iaitu kromatografi cecair /spektrometri jisim masa penerbangan (LC-TOF/MS). Pengoptimuman SPE dilakukan terhadap jenis pengerap, pelarut elusi dan kadar aliran sampel untuk mendapatkan perolehan semula yang baik memandangkan sifat-sifat fizikokimia sebatian sasaran yang berbeza dari segi nilai pKa dan logKow. Kepilihan pengukuran TOF ditingkatkan, selang jisim yang sempit dan tepat digunakan untuk membina semula kromatografi surih. Ion kromatografi pada kebiasaannya diekstrak mengunakan tetingkap jisim 20 mDa bagi ke semua sebatian sasaran. Walaubagaimanapun, penurunan tetingkap jisim dari 500 kepada 200 mDA menghasilkan hamper dua hingga empat kali peningkatan nisbah isyarat kepada hingar. Kaedah ini telah ditentusahkan terhadap air minuman (AM), air permukaan (AP), influen dan efluen loji rawatan kumbahan (STP) dan hospital (HSP). Had pengesanan instrumen (μg/L) ialah 5, 1.5, 0.8, 1.5, 0.8, 0.3, 5, 0.8, 3, 5 dan 1.5 masing - masing bagi kafein, prazosin, enalapril, carbamazepine, nifedipine, gliclazide, levonorgestrel, simvastatin, hydrochlorothiazide, diclofenac-Na danasidmefenamic. Had kuantifikasi (LOQ) adalah serendah 0.4, 1.6, 5, 2.9, 2.2 dan 11 ng/L masing - masing bagi AM, AP, influen dan efluen HSP dan loji rawatan air kumbahan. Secara purata, perolehan semula yang baik iaitu melebihi 70% di perolehi bagi kebanyakan analit sasaran di dalam semua matriks. Kesan matriks telah dinilai terhadap semua jenis sampel. Kaedah yang dicadang telah berjaya digunapakai bagi penentuan sebatian sasaran di dalam sisa air mentah dan terawat dari empat buah loji rawatan air kumbahan dan tiga hospital di Malaysia, serta dua titik persampelan air permukaan. Hasil kajian menunjukkan bahawa beberapa sebatian dikaji iaitu kafein, carbamazepine, gliclazide, simvastatin, hydrochlorothiazide dan asid mefenamik mempunyai tahap kekalan sederhana ke tinggi di dalam efluen rawatan kumbahan dan juga di dalam sungai. Kekerapan pengesanan semua sebatian bagi semua titik persampelan bagi tempoh sembilan bulan pemantauan (dari April hingga Disember 2013) yang melibatkan 105 sampel adalah seperti berikut: kafein 81% (85:105), prazosin 47% (49:105), enalpril 24% (25:105), carbamazepine 78% (82:105), gliclazide 92.7% (89:96), levonorgestrel 27.6% (29:105), simvastatin 40% (42:105), hydrochlorothiazide 81% (85:105), diclofenac-Na 32.4% (34:105) dan asid mefenamik 56.2% (59:105). Nifedipine telah dikesan hanya dua kali daripada 105 sampel yang dianalisis. Min kepekatan farmaseutikal yang dikesan bagi influen dan efluen STP, influen dan efluen hospital serta air permukaan masing - masing adalah dari julat ˂ LOQ hingga 3700 ng/L, 11 hingga 577 ng/L, 19 hingga 1419 ng/L, 19 ke 1468 ng/L dan 6 hingga 475 ng/L. Kepekatan tertinggi dikesan bagi kesemua titik persampelan adalah kafein iaitu 9099 ng/L. Analisis multivariat melibatkan analisis kelompok, analisis komponen prinsipal dan analisis diskriminan telah digunapakai untuk menilai kehadiran farmaseutikal di dalam sampel air. Keputusan kajian mendedahkan bahawa prazosin dan gliclazide dikesan buat kali pertama dalam persekitaran akuatik. Kajian ini telah membuktikan bahawa persekitaran akuatik Malaysia mengandungi pelbagai sisa farmaseutikal pada tahap yang berbeza-beza.,Ph.D | - |
| dc.language.iso | eng | - |
| dc.publisher | UKM, Bangi | - |
| dc.relation | Faculty of Science and Technology / Fakulti Sains dan Teknologi | - |
| dc.rights | UKM | - |
| dc.subject | Pharmaceutical | - |
| dc.subject | Liquid chromatography | - |
| dc.subject | Mass spectrometry | - |
| dc.subject | Liquid chromatography. | - |
| dc.title | Multi-residue analyticalmethodology based on liquid chromatography-time-of-flight-mass spectrometry for the analysis of pharmaceutical residues in aquatic samples | - |
| dc.type | Theses | - |
| dc.format.pages | 189 | - |
| dc.identifier.callno | QD79.C454 Q338 2015 | - |
| dc.identifier.barcode | 001461 | - |
| Appears in Collections: | Faculty of Science and Technology / Fakulti Sains dan Teknologi | |
Files in This Item:
| File | Description | Size | Format | |
|---|---|---|---|---|
| ukmvital_81691+SOURCE1+SOURCE1.0.PDF Restricted Access | 8.54 MB | Adobe PDF |  View/Open |
Items in DSpace are protected by copyright, with all rights reserved, unless otherwise indicated.