title: Low density solvent based dispersive liquid-liquid microextraction with gas chromatography-electron capture detection for the determination of cypermethrin in tissues and blood of cypermethrin treated rats.
abstract: A simple and rapid method to determine the cypermethrin (CYP) insecticide in rat tissues (kidney, liver and brain) and blood has been developed for the first time using low density solvent-dispersive liquid-liquid microextraction (LDS-DLLME) followed by gas chromatography-electron capture detector (GC-ECD) analysis. Initially, tissue samples containing CYP were homoginized in acetone. Subsequently, homogenate was mixed with n-hexane (extraction solvent) and the mixture was rapidly injected into water. The upper n-hexane layer was collected in a separate microtube and injected into GC-ECD for analysis. Blood samples were diluted with ultrapure water and subjected to DLLME through similar procedure. Parameters such as type and volume of disperser and extraction solvent, salting out effect and extraction time, which can affect the extraction efficiency of DLLME, were optimized. Method was validated by investigating linearity, precision, recovery, limit of detection (LOD) and quantification (LOQ). LODs in tissue were in the range of 0.043-0.314 ng mg(-1) and for blood it was 8.6 ng mL(-1) with a signal to noise ratio of 3:1. LOQs in tissue were in the range of 0.143-1.03 ng mg(-1) and for blood it was 28.3 ng mL(-1) with a signal to noise ratio of 10:1. Mean recoveries of CYP at three different concentation levels in all the matrices were found to be in the range of 81.6-103.67%. The results show that, LDS-DLLME coupled with GC-ECD offers a simple, rapid and efficient technique for extraction and determination of CYP in rat tissues and blood samples, which in turn would be useful for toxicological studies of CYP.
authors.affiliation: Analytical Chemistry Section, CSIR-Indian Institute of Toxicology Research, PO Box 80, M G Marg, Lucknow 226 001, India. mohanitrc@gmail.com
authors.forename: Mohana Krishna Reddy
authors.initials: MK
authors.lastname: Mudiam
authors.forename: Rajeev
authors.initials: R
authors.lastname: Jain
authors.forename: Shailendra Kumar
authors.initials: SK
authors.lastname: Maurya
authors.forename: Haider A
authors.initials: HA
authors.lastname: Khan
authors.forename: Sanghamitra
authors.initials: S
authors.lastname: Bandyopadhyay
authors.forename: R C
authors.initials: RC
authors.lastname: Murthy
mesh_terms: D000096:Acetone; D000818:Animals; D001923:Brain Chemistry; D002849:Chromatography, Gas / Q000379:methods*; D006586:Hexanes; D006863:Hydrogen-Ion Concentration; D007668:Kidney / Q000737:chemistry; D057230:Limit of Detection; D059627:Liquid Phase Microextraction / Q000379:methods*; D008099:Liver / Q000737:chemistry; D008297:Male; D009994:Osmolar Concentration; D011722:Pyrethrins / Q000032:analysis* / Q000097:blood*; D051381:Rats; D017208:Rats, Wistar; D015203:Reproducibility of Results
chemical_list: D006586:Hexanes; D011722:Pyrethrins; D000096:Acetone; C017160:cypermethrin; C026385:n-hexane