Matrix Solid Phase Dispersion‐Accelerated Solvent Extraction for Determination of OCP Residues in Fish Muscles

Abstract

A rapid, sensitive and accurate matrix solid phase dispersion-accelerated solvent extraction (MSPD-ASE) method for selective determination of sixteen organochlorine pesticide (OCP) residues in fish samples has been developed and validated. 2 g fresh fish muscle was dispersed with 10 g anhydrous sodium sulfate and 2 g acid alumina thoroughly, and loaded into the stainless-steel extraction cell containing 6 g of acid alumina and 10 g anhydrous sodium sulfate. The temperature 60°C and two extraction cycles of 5 min gave adequate extraction efficiency using DCM-hexane (3:7, v/v) mixture as solvent. Not only the lipids, but also other co-extracts, which peaks mostly located in the forepart of chromatograms and maybe interfere the identification or quantitation of analytes, were eliminated exhaustively, while analytes were extracted selectively. Sixteen OCPs were identified by retention time of standards and quantified using mirex as internal standards. These detected OCPs were confirmed by GC-MS in real samples. The performance of proposed method was evaluated and validated: the detection limits were 0.008-0.05 ng g -1 , relative standard deviations were 1.9-5.0%, and recoveries were 91.0-104.1% spiked at 10 ng g -1 level. The accuracy and precision of proposed method were equal to or better than that of traditional Soxhlet extraction method.

Study of vortex-assisted MSPD and LC-MS/MS using alternative solid supports for pharmaceutical extraction from marketed fish

“…Results showed that 1:1 (the lowest level) was the best ratio. This result is similar to the one reported by Shen et al [47] who found a 1:1 ratio by employing MSPD for the extraction of organochlorine pesticides from fish samples and determination by GC-ECD and GC-MS. Recoveries ranged from 82 to 106 % with RSD lower than 6 %. The same ratio was not verified by Fan et al [48] who concluded that a 1:3 ratio showed the best results for the extraction of steroid hormones from animal-origin food with determination by LC-MS/MS.…”

Supercritical fluid extraction followed by nanostructured supramolecular solvent extraction for extraction of levonorgestrel and megestrol from whole blood samples

“…This is while it was reported that addition A c c e p t e d M a n u s c r i p t 9 of NaCl decreases the efficiency of dispersion of extraction phase and mass transfer in aqueous medium, leading to a decrease in extraction efficiency. To investigate the influence of salt addition on performance of SUPRASF extraction, various experiments were performed by adding different amounts of NaCl (0-20% w/v) to the sample solution.…”

“…Also, owing to the fact that sorbents are nonselective, further purification of the extracts is often still required to remove coextractants before further analysis. Shen et al reported combination of MSPD with accelerated solvent extraction (ASE) from soil samples and fish muscle for determination of OCP residues [9,10]. However, the consumption of hazardous organic solvents in ASE is relatively high, the final extract needs solvent evaporation; and extraction of other matrix interferences is probable, which reduces higher purification of extract.…”

“…From the first introduction of MSPD in 1989 by Barker, it has found increasing acceptance in trace analysis of organic compounds using chromatographic techniques due to providing sample homogenization, extraction, and clean up in one step [6][7][8]. Until now, MSPD in combination with chromatography methods has been successfully applied for determination of different analytes in various biological samples [9][10][11][12][13][14][15][16][17][18][19][20].…”

Methodologies and Results Concerning the Determination of Ocs And Pcbs From Fish Meat

“…The sample preparation for extraction is simple and rapid, the high pressure during extraction allows the recovery of thermally labile analytes even at high temperatures and numerous samples can be extracted in one cycle. Extract clean-up is usually necessary due to one major drawback of the method-the presence of a large amount of coextracted interferences which must be separated from analytes, or chromatographic performance will seriously deteriorate (Shen et al, 2011).…”