Ultrasonication followed by single‐drop microextraction combined with GC/MS for rapid determination of organochlorine pesticides from fish

Abstract

A novel, rapid and simple sample pretreatment technique termed ultrasonication followed by single-drop micro-extraction (U-SDME) has been developed and combined with GC/MS for the determination of organochlorine pesticides (OCPs) in fish. In the present work, the lengthy procedures generally used in the conventional methods like, Soxhlet extraction, supercritical fluid extraction, pressurized liquid extraction and microwave assisted solvent extraction for extraction of OCPs from fish tissues are minimized by the use of two simple extraction procedures. Firstly, OCPs from fish were extracted in organic solvent with ultrasonication and then subsequently preconcentrated by single-drop micro-extraction (SDME). Extraction parameters of ultrasonication and SDME were optimized in spiked sample solution in order to obtain efficient extraction of OCPs from fish tissues. The calibration curves for OCPs were found to be linear between 10-1000 ng/g with correlation of estimations in the range 0.990-0.994. The recoveries obtained in blank fish tissues were ranged from 82.1 to 95.3%. The LOD and RSD for determination of OCPs in fish were 0.5 ng/g and 9.4-10.0%, respectively. The proposed method was applied for the determination of bioconcentration factor in fish after exposure to different concentrations of OCPs in cultured water. The present method avoids the co-extraction of lipids, long extraction steps (>12 h) and large amount of organic solvent for the separation of OCPs. The main advantages of the present method are rapid, selective, sensitive and low cost for the determination of OCPs in fish.

Development and applications of single‐drop microextraction for pesticide residue analysis: A review

“…Ye et al [27] also reported similar observation and recommended that HA concentration must be less than 50 mg/L. Shrivas and Wu [29] described ultrasonication followed by SDME combined with GC-MS for rapid determination of OCPs in fish sample. They analyzed OCPs from fish tissue by spiking 1.0 g of fish tissue followed by ultrasonication with water-miscible solvents.…”

Determination of Polychlorinated Biphenyls in Fish Tissues from Shanghai Seafood Markets Using a Modified QuEChERS Method

“…As in the previous results, this supports the notion that the polar features could be very similar to PCBs found in fish tissue. [5][6][7][8][9][10][11][12][13][14][15][16][17][18][19][20] Moreover, the ice-cold condition was strongly suggested to remove the heat disturbance.…”

“…4,[12][13][14][15] In addition, GPC, ASE, soxhlet, ultrasonic extraction and single-drop were also used to promote extraction efficiency from fish several years ago. 4,10,14,[16][17][18][19] Moreover, researchers have focused on simplified and rapid determination of PCBs, such as by using screening, programmable temperature vaporization-large volume injection (PTV-LVI) or high throughput methods. Most literature have focused on six PCBs (IUPAC Nos.…”

The development and optimization of a modified single-drop microextraction method for organochlorine pesticides determination by gas chromatography-tandem mass spectrometry

“…Different organic solvents, namely toluene, iso-octane, chloroform and n-hexane, are frequently used in SDME, as the acceptor phase, of liquid drop to extract the pesticides from aqueous solution [3,39]. After three replicate analysis, the chromatographic signals obtained from the analytes using nhexane as the acceptor phase, are approximately two times higher than the signals obtained with dichloromethane and tetrachloromethane.…”

“…Ahmadi et al employed some modification of the needle tip, causing its cross section to increase and increasing adhesion force between the needle tip and the drop, thereby increasing drop stability and achieving a higher stirrer speed (up to 1,700 rpm) [30]. SDME in pesticide residues analysis has been applied with success in both liquid water [27,30,31], juices [32,33], wine [34,35], oils [36] and solid samples (vegetables [24,37,38], fish [39] by providing low limits of detection and high selectivity as compared with classic robust sample preparation techniques. The novel approachs of SDME were developed by different authors.…”