title: Combination of solid-phase extraction with dispersive liquid-liquid microextraction followed by GC-MS for determination of pesticide residues from water, milk, honey and fruit juice.
abstract: In this work, an effective preconcentration method for the extraction and determination of traces of multi-residue pesticides was developed using solid-phase extraction (SPE) coupled with dispersive liquid-liquid microextraction and gas chromatography-mass spectrometry (GC-MS). Variables affecting the performance of both extraction steps such as type and volume of elution and extraction solvents, breakthrough volume, salt addition, extraction time were thoroughly investigated. The proposed method resulted in good linearities (R(2)>0.9915) over the ranges of 1-10,000ngkg(-1), limits of detection (LODs) in the range of 0.5-1.0ngkg(-1) at S/N=3, and precision of RSD% of ⩽11.8. Under optimal conditions, the preconcentration factors were obtained in the range of 2362-10,593 for 100mL sample solutions. Comparison of the proposed method with other ones demonstrated that SPE-DLLME method provides higher extraction efficiency and larger preconcentration factor for determination of pesticides residues. Further, it is simple, inexpensive, highly sensitive, and can be successfully applied to separation, preconcentration and determination of the pesticides (and other noxious materials) in different real food samples.
authors.affiliation: Department Chemistry, Razi University, Kermanshah, Iran. Electronic address: mshamsipur@yahoo.com.
authors.forename: Mojtaba
authors.initials: M
authors.lastname: Shamsipur
authors.affiliation: Department Chemistry, Razi University, Kermanshah, Iran; Iranian Research and Development Center for Chemical Industries, ACECR, Tehran, Iran.
authors.forename: Najmeh
authors.initials: N
authors.lastname: Yazdanfar
authors.affiliation: Iranian Research and Development Center for Chemical Industries, ACECR, Tehran, Iran.
authors.forename: Mahnaz
authors.initials: M
authors.lastname: Ghambarian
mesh_terms: D000818:Animals; D002417:Cattle; D005618:Fresh Water / Q000737:chemistry*; D000067030:Fruit and Vegetable Juices / Q000032:analysis*; D008401:Gas Chromatography-Mass Spectrometry / Q000379:methods*; D006722:Honey / Q000032:analysis*; D057230:Limit of Detection; D059627:Liquid Phase Microextraction / Q000379:methods*; D008892:Milk / Q000737:chemistry*; D010573:Pesticide Residues / Q000737:chemistry / Q000302:isolation & purification*; D052616:Solid Phase Extraction / Q000379:methods*
chemical_list: D010573:Pesticide Residues
keywords: Aldrin (PubChem CID: 12310947); Carbaryl (PubChem CID: 6129); Dispersive liquid–liquid microextraction; Ethion (PubChem CID: 3286); Fenitrothion (PubChem CID: 31200); Fenpropathrin (PubChem CID: 47326); Food sample analysis; Gas chromatography–mass spectrometry; Malathion (PubChem CID: 4004); Metalaxyl (PubChem CID: 42586); Multi-residue pesticides; Permethrin (PubChem CID: 40326); Solid-phase extraction; Tetradifon (PubChem CID: 8305)