Sains Malaysiana 42(2)(2013): 149–157

Application of Dispersive Liquid-liquid Microextraction Based on Solidification

of Floating Organic Droplet to the Analysis of Antidepressant Drugs in Water Samples

(Aplikasi Pengekstrakan Cecair-cecair Serakan Berdasarkan Pemejalan Titisan Organik Terapung dalam Analisis Dadah Anti-Kemurungan di dalam Sampel Air)

Mohd Marsin Sanagi^1,2* Siti Umairah Mokhtar², & Wan Aini Wan Ibrahim^1,2

& Hassan Y. Aboul-Enein³

¹Ibnu Sina Institute for Fundamental Science Studies, Universiti Teknologi Malaysia

81310 Johor Bahru, Malaysia

²Department of Chemistry, Faculty of Science, Universiti Teknologi Malaysia

81310 Johor Bahru, Malaysia

³Department of Pharmaceutical and Medicinal Chemistry, National Research Centre

Dokki, 12311, Cairo, Egypt

Received: 11 May 2012 / Accepted: 13 August 2012

ABSTRACT

A simple and rapid sample preparation method based on dispersive liquid-liquid microextraction-solidification of floating organic drop (DLLME-SFO) combined with gas chromatography-mass spectrometry (GC-MS) method was developed for the analysis of antidepressant drugs in water samples. This method uses organic solvent with low density and less toxicity. In the method, the disperser solvent (0.5 mL acetonitrile) containing 30 μL of n-hexadecane was rapidly injected using a syringe into 5.0 mL of water sample in a glass tube. After centrifugation for 7 min at 3500 rpm, the mixture was cooled in ice bath for 5 min. The solidified n-hexadecane was transferred into a conical vial, where it melted rapidly at room temperature and 2 μL of it was injected into a gas chromatograph for analysis. Under optimized conditions, the method showed good linearity in the range of 0.04 - 0.12 μg mL^-1 for amitriptyline and chlorpromazine with correlation of determination (r²) in the range of 0.992 - 0.995. The limits of detections (LODs) were in the range 0.0085 - 0.0285 μg mL^-1. The extraction recoveries of amitriptyline and chlorpromazine from water samples at spiking level of 0.08 μg mL^-1 were 71.34 - 73.52% and 73.83 - 91.09%, respectively, with relative standard deviations (RSDs) in the range of 4.97 - 6.85% for amitriptyline and 4.84 - 7.49% for chlorpromazine. The method was successfully applied to the determination of the analytes in drinking water, lake water and tap water samples.

Keywords: Antidepressant drugs; dispersive liquid-liquid microextraction-solidification of floating organic; gas chromatography-mass spectrometry; water samples

ABSTRAK

Satu kaedah penyediaan sampel yang ringkas dan cepat berdasarkan pengekstrakan mikro cecair-cecair penyerakan pemejalan titisan organik terapung (DLLME-SFO) bergabung dengan kromatografi gas-spektrometri jisim (GC-MS) telah dibangunkan untuk analisis dadah anti-kemurungan di dalam sampel air. Dalam kaedah ini, pelarut penyebar (0.5 mL asetonitril) yang mengandungi 30 μL n-heksadekana disuntik dengan cepat menggunakan picagari ke dalam 5.0 mL air dalam tiub kaca. Larutan diemparkan selama 7 min pada 3500 rpm, tiub kaca direndam di dalam kukus ais untuk langkah penyejukan selama 5 min, pelarut pepejal n-heksadekana dipindahkan ke dalam tiub berbentuk kon, dan ia akan melebur dengan cepat pada suhu bilik dan 2 μL cecair itu disuntik ke dalam kromatografi gas untuk dianalisis. Beberapa parameter DLLME-SFO dikenal pasti, termasuk jenis dan isi padu pelarut pengekstrakan dan pelarut penyebar, masa pengekstrakan dan kesan garam. Dalam keadaan optimum, kaedah ini menunjukkan kelinearan yang baik dalam julat 0.04 - 0.12 μg mL^-1 untuk amitriptilina dan klorpromazina dengan kolerasi penentuan (r²) dalam julat 0.992 - 0.995. Had pengesanan (LODs) adalah dalam julat 0.0085 - 0.0285 μg mL^-1. Keboleh-pulangan pengekstrakan untuk amitriptilina dan klorpromazina daripada sampel air pada tahap campuran 0.08 μg mL^-1 adalah masing-masing 71.34 -73.52% dan 73.83 - 91.09% dengan sisihan piawai relatif (RSDs) dalam julat 4.97 - 6.85% untuk amitriptilina dan 4.84 - 7.49% untuk klorpromazina. Kaedah ini berjaya diaplikasikan bagi pengesanan dadah anti kemurungan dalam sampel air minuman, air tasik dan air paip.

Kata kunci: Dadah anti-kemurungan; kromatografi gas-spektrometri jisim; pengekstrakan mikro cecair-cecair penyerakan pemejalan titisan organik terapung; sampel air

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*Corresponding author; email: marsin@kimia.fs.utm.my