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)

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*Corresponding author; email: nfaizah@ukm.edu.my

 

 

 

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