Viable and Rapid Determination of Organochlorine Pesticides in Water

Abstract

Vortex-assisted liquid-liquid microextraction (VALLME) procedure was developed for the determination of different organochlorine pesticides (OCPs) in water samples by GC-MS. After the determination of the most suitable extraction solvent and rotational speed of the vortex, parameters such as vortex extraction time, solvent volume, ionic strength of the sample were optimized by using a 2 3 factorial experimental design. The optimized extraction conditions for 5 mL water sample were as follows: extraction solvent, bromoform; solvent volume, 50 mL; vortex extraction time, 2 min at 3000 rpm with no ionic strength adjustment, centrifugation 5 min at 4000 rpm. Limits of detection (LODs) and quantification (LOQs) were in the range of 0.011-0.052 and 0.037-0.173 mg/L, respectively. Mean recoveries of OCPs from fortified water samples are 96% for three different fortification levels between 0.1 and 5 mg/L and relative standard deviations of the recoveries are below 6%. The performance of the developed method was compared with traditional liquid-liquid extraction on real water samples including tap water, well water, surface (lake and stream) water, municipal wastewater, and treated municipal wastewater and comparable extraction efficiencies were obtained. The proposed VALLME procedure requires small volumes of solvent and water sample. It is viable, rapid, and easy to use for the determination of OCPs in water samples by using GC-MS.

Analyses of polychlorinated biphenyls in waters and wastewaters using vortex‐assisted liquid–liquid microextraction and gas chromatography‐mass spectrometry

“…In vortex‐assisted extraction, extraction solvent should be water immiscible and it should remain at the bottom or surface of the centrifuge tube. Moreover, the chosen extraction solvent presents good affinity for target compounds, and it should have excellent gas chromatographic behavior and high extraction capability for interesting analytes 33, 34, 37, 40–42. Therefore, different extraction solvents denser than the water (dichloromethane, chloroform, 1,2‐dichlorobenzene, and bromoform) and lower than the water ( n ‐hexane, cyclohexane, ethyl acetate, petroleum ether, 2‐propanol, isooctane, n ‐pentane, toluene, diethyl ether, and 1‐octanol) were examined.…”

“…They used this new microextraction technique for the determination of trace amount of octylphenol, nonylphenol, and bisphenol‐A in water samples. In addition, this method was optimized and used for the residue analysis of organochlorine pesticides in water and wastewater samples 37. They demonstrate that VALLME is a fast, repeatable, and efficient method and it requires quite small volume of extraction solvent and water sample.…”

Levels of Organochlorine Pesticides and Heavy Metals in Surface Waters of Konya Closed Basin, Turkey

“…The temperature of the ion source and MS transfer line were maintained at 170°C and 280°C, respectively. The oven program for OCPs was the same as reported by Ozcan [16]. MS detector was operated in selected ion monitoring (SIM) mode.…”

Analytical Methods for Viable and Rapid Determination of Organochlorine Pesticides in Water and Soil Samples

“…Consequently, residue analyses of OCPs in waters and soils by developing analytical procedure continue to be an active area of research in recent years (Santos & Galceran, 2004). Trace analysis of OCPs in water is usually performed by gas chromatography (GC) combined with a previous an extraction or a pre-concentration step including traditional liquid-liquid extraction (LLE) (Barcelo´, 1993, Fatoki & Awofolu, 2003Tahboub et al, 2005), solid phase extraction (SPE) (Aguilar et al, 1996;, solid phase microextraction (SPME) (Page & Lacroix, 1997;Aguilar et al, 1999;Tomkins & Barnard, 2002;Li et al, 2003;Dong et al, 2005) and the more recently developed liquid phase microextraction under different names, i.e., dispersive liquid-liquid microextraction (DLLME) (Cortada et al, 2009a;Leong & Huang, 2009;Tsai & Huang, 2009), liquid-phase microextraction (LPME) (Huang & Huang, 2007;Farahani et al, 2008), single-drop microextraction (SDME) (Cortada et al, 2009b), polymer-coated hollow fiber microextraction (PC-HFME) (Basheer et al, 2004), stir bar sorptive extraction (SBSE) (Leo´n et al, 2003;Pe´rez-Carrera et al, 2007), ultrasound assisted emulsification-microextraction (USAEME) (Ozcan et al, 2009a), vortex assisted liquid-liquid microextraction (VALLME) (Ozcan, 2010). Among these methods, LLE and SPE are the oldest procedures for the extraction of OCPs from aqueous matrices.…”

“…USAEME procedure combines micro-extraction system and ultrasonic radiation in one step. Ultrasonic radiation is a powerful means for acceleration of various steps in analytical procedure for both solid and liquid samples (Priego-Lo´pez & Luque de Castro, 2003;Aydin et al, 2006;Tor et al, 2006a;2006b;Ozcan et al, 2009a;2009c;2010). USAEME technique leads to an increment in the extraction efficiency in a minimum amount of time (Luque de Castro & Priego-Capote, 2006;.…”