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 Sanagi1,2* Siti Umairah Mokhtar2, & Wan Aini Wan Ibrahim1,2

& 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

 

Diserahkan: 11 Mei 2012 / Diterima: 13 Ogos 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

RUJUKAN

 

Adams, M. 2004. Antidepressant drugs found in drinking water; pharmaceuticals have now become environmental pollutants. Accessed on line at: http://www.naturalnews.com/001891.html (27 July 2012).

Asadollah, T., Dadfarni, S. & Shabani, A.M.H. 2010. Separation/preconcentration and determination of vanadium with dispersive liquid–liquid microextraction based on solidification of floating organic drop (DLLME-SFO) and electrothermal atomic absorption spectrometry. Talanta 82: 208–212.

Es’haghi, Z. 2009. Determination of widely used non-steroidal anti-inflammatory drugs in water samples by in situ derivatization, continuous hollow fiber liquid-phase microextraction and gas chromatography flame ionization detector. Analytica Chimica Acta 64: 83-88.

Esrafili, A., Yamini, Y. & Shariati, S. 2007. Hollow fiber-based liquid phase microextraction combined with high-performance liquid chromatography for extraction and determination of some antidepressant drugs in biological fluids. Analytica Chimica Acta 604: 127-133.

Kevin, J.B., Jim, T.Y., Mehmet, C., Edward, J.B. & Roberts, L. 2010. Trace determination of pharmaceuticals and other wastewater-derived micropollutants by solid phase extraction and gas chromatography/mass spectrometry. Journal of Chromatography A 1217: 558-564.

Leong, M.I. & Shang, D.H. 2008. Dispersive liquid–liquid microextraction method based on solidification of floating organic drop combined with gas chromatography with electron capture or mass spectrometry detection. Journal of Chromatography A 1211: 8-12.

Mirzaei, M., Behzadi, M., Abadi, N.M. & Beizaei, A. 2011. Simultaneous separation preconcentration of ultra trace heavy metals in industrial wastewaters by dispersive liquid–liquid microextraction based on solidification of floating organic drop prior to determination by graphite furnace atomic absorption spectrometry. Journal of Hazardous Material 186: 1739-1743.

Rezaee, M., Assadi, Y., Hosseini, M.R.M., Aghaee, E., Ahmadi, F. & Berijani, S. 2006. Determination of organic compounds in water using dispersive liquid–liquid microextraction. Journal of Chromatography A 1116: 1-9.

Sobhi, H.R., Yamini, Y. & Abadi, R.H.H.B. 2007. Extraction and determination of trace amounts of chlorpromazine in biological fluids using hollow fiber liquid phase microextraction followed by high-performance liquid chromatography. Journal of Pharmaceutical and Biomedical Analysis 45: 769-774.

Tatsuo, S., Masaru, T. & Einosuke, T. 2006. Solid-phase extraction and analysis of 20 antidepressant drugs in human plasma by LC/MS with SSI method. Forensic Science International 162:108-112.

Yamini, Y., Rezaee, M., Khanchi, A., Faraji, M. & Saleh, A. 2010. Dispersive liquid–liquid microextraction based on the solidification of floating organic drop followed by inductively coupled plasma-optical emission spectrometry as a fast technique for the simultaneous determination of heavy metals. Journal of Chromatography A 1217: 2358-2364.

 

*Pengarang untuk surat-menyurat; email: marsin@kimia.fs.utm.my

 

 

 

sebelumnya