 |
 |
 |
 |
 |
 |
Sains Malaysiana 47(5)(2018): 931–940 http://dx.doi.org/10.17576/jsm-2018-4705-08
Pengoptimuman Kaedah dan Analisis Farmaseutik dalam Air Kumbahan dan Air Sungai
(Optimisation of Analytical Method and Analysis of Pharmaceuticals in Sewage and River Water)
NURFAIZAH ABU TAHRIM1,2*, MD. PAUZI ABDULLAH3 & YANG FARINA ABDUL AZIZ1
1Pusat Pengajian Sains Kimia & Teknologi Makanan, Fakulti Sains dan Teknologi, Universiti Kebangsaan Malaysia, 43600 UKM Bangi,
Selangor Darul Ehsan, Malaysia
2Pusat Penyelidikan dan Analisis Air (ALIR), Fakulti Sains dan Teknologi, Universiti Kebangsaan Malaysia, 43600 UKM Bangi, Selangor Darul Ehsan, Malaysia
3Akademi Sains Malaysia, Tingkat 20, Sayap Barat, Menara MATRADE, Jalan Sultan Haji Ahmad Shah, 50480
Kuala Lumpur, Wilayah Persekutuan, Malaysia
Received: 16 September
2017/Accepted: 2 January 2018
ABSTRAK
Loji rawatan kumbahan (STP) sedia ada khususnya di Malaysia tidak direka untuk menyingkirkan bahan farmaseutik yang tergolong dalam kategori bahan cemar baru muncul. Oleh kerana farmaseutik yang hadir dalam persekitaran akuatik ialah pada kepekatan yang sangat rendah iaitu dalam julat bahagian per bilion dan trilion, satu kaedah pengekstrakan dan analisis yang peka perlu dibangunkan. Dalam kajian ini, kaedah analisis berdasarkan pengekstrakan fasa pepejal (SPE) diikuti dengan kromatografi cecair-spektrometri jisim masa penerbangan (LC-TOF-MS) menggunakan mod pengionan secara semburan elektro positif telah berjaya dibangunkan untuk menentukan kehadiran sepuluh farmaseutik terpilih dalam air kumbahan dan air sungai. Farmaseutik yang dikaji termasuk acetaminophen, theophylline, caffeine, metoprolol, sulfamethoxazole,
carbamazepine, prednisolone, ketoprofen, norgestrel dan simvastatin. Kaedah SPE menggunakan langkah pengekstrakan tunggal yang menggunakan isi padu sampel yang rendah sebanyak 100 mL dan pelarut elusi yang minimum telah berjaya dicapai. Peratus perolehan semula untuk kesemua farmaseutik dalam sampel air sungai berada dalam julat 54-99% manakala bagi sampel efluen STP pula berada dalam julat 57-96%. Jangka masa analisis LC-TOF-MS termasuk masa imbangan adalah selama 25 min dengan menggunakan suntikan sampel 20 μL. Prosedur SPE bersama-sama dengan kaedah analisis yang telah dibangunkan menghasilkan had kuantifikasi (LOQ) dalam lingkungan 0.031-0.882 μg/L untuk sampel STP dan 0.030-0.926 μg/L untuk sampel air sungai.
Kata kunci: Farmaseutik; loji rawatan kumbahan; pengekstrakan fasa pepejal (SPE)
ABSTRACT
Sewage treatment
plants (STPs) particularly in Malaysia are not designed to
eliminate pharmaceuticals which belong to the category of emerging
contaminants. Considering the levels of these contaminants could be incredibly
low which are in the range of parts per billion and trillion in the aquatic
environment, very sensitive analytical techniques and extraction methodologies
have to be developed. In this present work, an analytical method based on solid
phase extraction (SPE) followed by liquid
chromatography-time-of-flight mass spectrometry (LC-TOF-MS)
in positive electrospray ionisation mode was
successfully developed to determine the presence of ten selected
pharmaceuticals in aquatic environment. The compounds under study include
acetaminophen, theophylline, caffeine, metoprolol, sulfamethoxazole,
carbamazepine, prednisolone, ketoprofen, norgestrel and simvastatin. The SPE procedure
was successfully achieved with a single extraction step using a low sample
volume of 100 mL and minimum volume of eluting solvent. Percentage recovery for
all pharmaceuticals in river water samples were in the range of 54-99% while
for STP effluent samples were in the range of 57-96%. The
total run time inclusive of equilibration in LC-TOF-MS analysis
was 25 min with sample injection volume of 20 μL.
The application of the optimised SPE procedure
together with the instrumental analysis resulted in limit of quantification (LOQ)
of 0.031 - 0.882 μg/L and 0.030 - 0.926 μg/L in STP and river water samples, respectively.
Keywords: Pharmaceuticals; sewage treatment plant; solid phase
extraction (SPE)
REFERENCES
Albert, O., Desdoits-Lethimonier, C., Lesné, L., Legrand, A., Guillé,
F., Bensalah, K., Dejucq-Rainsford,
N. & Jégou, B. 2013. Paracetamol, aspirin and indomethacin display endocrine disrupting properties
in the adult human testis in vitro. Human Reproduction 28(7):
1890-1898.
Al-Odaini, N.A., Zakaria, M.P., Yaziz, M.I. & Surif, S. 2010. Multi-residue analytical method for human pharmaceuticals and
synthetic hormones in river water and sewage effluents by solid-phase
extraction and liquid chromatography-tandem mass spectrometry. Journal
of Chromatography A1217(44): 6791-6806.
Al-Qaim, F.F., Abdullah, M.P., Othman,
M.R., Latip, J. & Zakaria,
Z. 2014. Multi-residue analytical methodology-based
liquid chromatography-time-of-flight-mass spectrometry for the analysis of
pharmaceutical residues in surface water and effluents from sewage treatment
plants and hospitals. Journal of Chromatography A 1345: 139-153.
Al-Qaim, F.F., Abdullah, M.P., Latip, J., Khalik, W.M.A.W.M., Tahrim, N.A., Abidin, N.A.Z.
& Othman, M.R. 2016. Detection of gliclazide in aqueous samples using liquid chromatography/time-of-flight/mass
spectrometry. Sains Malaysiana45(5): 803-810.
Bienkowski, B. 2015. Bacteria
May Be Remaking Drugs in Sewage. Environmental Health
News. https://www.
scientificamerican.com/article/bacteria-may-be-remaking-drugs-in-sewage/. Diakses pada 20 April 2017.
González-Barreiro, C., Lores, M., Casais, M.C. & Cela, R. 2003. Simultaneous determination of neutral and acidic pharmaceuticals in wastewater
by high-performance liquid chromatography-post-column photochemically induced fluorimetry. Journal of Chromatography A993(1-2): 29-37.
Gros, M., Petrovic, M. & Barceló, D. 2006. Development of a multi-residue analytical methodology based on liquid
chromatography-tandem mass spectrometry (LC-MS/MS) for screening and trace
level determination of pharmaceuticals in surface and wastewaters. Talanta 70(4): 678-690.
Lavén, M., Alsberg, T., Yu, Y., Adolfsson-Erici,
M. & Sun, H. 2009. Serial mixed-mode cation- and anion-exchange
solid-phase extraction for separation of basic, neutral and acidic
pharmaceuticals in wastewater and analysis by high-performance liquid
chromatography-quadrupole time-of-flight mass spectrometry. Journal
of Chromatography A1216(1): 49-62.
Ministry of Health Malaysia (MOH). 2014. Malaysian
Statistics on Medicine 2009-2010. The National Medicines
Use Survey.
National
Essential Drug List (NEDL). 3rd ed. 2012. http://www. pharmacy.gov.my/v2/sites/default/files/document-upload/ nedl-only-list publish-website.pdf.
Oropesa, A.L., Floro, A.M. & Palma, P.
2016. Assessment of the effects of the carbamazepine on the endogenous
endocrine system of Daphnia magna. Environmental Science and
Pollution Research 23(17): 17311-17321.
Petrovic, M., Gros, M. & Barcelo, D. 2006. Multi-residue analysis of pharmaceuticals in wastewater by
ultra-performance liquid chromatography-quadrupole-time-of-flight mass
spectrometry. Journal of Chromatography A1124(1-2):
68-81.
Sanagi, M.M., Mokhtar,
S.U., Ibrahim, W.A.W. & Aboul- Enein, H.Y. 2013. Application
of dispersive liquid-liquid microextraction based on
solidification of floating organic droplet to the analysis of antidepressant
drugs in water samples. Sains Malaysiana42(2): 149-157.
Tan, E.S.S., Ho, Y.B., Zakaria, M.P.,
Abdul Latif, P. & Saari, N. 2015. Simultaneous extraction and determination of pharmaceuticals and
personal care products (PPCPs) in river water and sewage by solid-phase
extraction and liquid chromatography-tandem mass spectrometry. International
Journal of Environmental Analytical Chemistry 95(9): 816-832.
U.S. EPA. 2008. Pharmaceuticals and Personal Care Products (PCPPs). http://water.epa.gov/scitech/swguidance/ppcp/ index.cfm. Diakses pada 3 Ogos 2016.
Vanderford, B.J. & Snyder,
S.A. 2006. Analysis of pharmaceuticals in water by isotope
dilution liquid chromatography/tandem mass spectrometry. Environmental Science and Technology 40(23): 7312-7320.
Vieno, N.M., Tuhkanen, T. & Kronberg, L.
2006. Analysis of neutral and basic pharmaceuticals
in sewage treatment plants and in recipient rivers using solid phase extraction
and liquid chromatography-tandem mass spectrometry detection. Journal
of Chromatography A1134: 101-111.
*Corresponding author; email: nfaizah@ukm.edu.my
|
|||
|
