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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
Diserahkan: 16
September 2017/Diterima: 2 Januari 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)
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*Pengarang
untuk surat-menyurat; email: nfaizah@ukm.edu.my
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