of 85–109% and MLODs were of 0.02–0.16 mg/kg [46]. Ionic liquid-linked dual
magnetic microextraction (IL-DMME) was developed as novel and facile extraction
technique for determination of pyrethroids in honey samples [45]. The method
consists of a combination of dispersive liquid-liquid microextraction (DLLME)
and dispersive microsolid-phase extraction using an ionic liquid ([C 6 MIM]NTf 2 )
and no-modified magnetic nanoparticles (S-BaFe), respectively [45]. Pyrethroids
were firstly extracted by the ionic liquid, and then the no-modified magnetic
nanoparticle was used to retrieve the ionic liquid containing the pyrethroids. Finally,
pyrethroids were extracted from nanoparticles by sonication using acetonitrile as
solvents. Recoveries were of 87–92% with MLODs of 0.03–0.05 μg/L [45]. Magnetic nanoparticles (MNPs) exhibit high selectivity and, in small amounts, can
provide high recovery of analytes, even from large-volume samples. They also
allow easy, rapid isolation of analytes using an external magnetic field. A competitive enzyme-linked immunosorbent assay (ELISA) method was employed for the
determination of cypermethrin and permethrin in agricultural products (wine, fruit,
and vegetable). No further cleanup was needed. Matrix interferences were minimized by diluting with phosphate-buffered saline containing 40% methanol
[48]. Recoveries were 74–99% with MLODs of 5–10 μg/kg [48]. QuEChERS
method was employed for extraction of pyrethroid pesticide residue from rice
grain [49]. Extraction was performed using acetonitrile, MgSO4, and NaCl. Recoveries were of 87–117% and MLODs were of 1 μg/kg [49]. SPME was employed for
extraction of pyrethroids from cucumber and watermelon samples using highperformance liquid chromatography combined with post-column photochemically
induced fluorimetry derivatization and fluorescence detector (HPLC-PIF-FD)
[50]. The optimum SPME conditions were extraction time 30 min, stirring rate
1,100 rpm, extraction temperature 65
C, sample pH 3, soaking time 7 min, desorption time 5 min, and acetonitrile content 25%. Recoveries were of 91–100% and
MLODs 1.3–5 μg/kg [50]. Liquid-liquid extraction of pyrethroids (cypermethrin and
deltamethrin) from pasteurized milk was performed using acetonitrile as extraction
solvent with cleanup by precipitation at low temperature without additional stages
for removal of fat interferences [51]. Recoveries were of 93% for cypermethrin and
84% for deltamethrin with MLODs of 7.5 ng/L [51]. From human breast milk,
pyrethroids were extracted by sonication with hexan/dichloromethane 2:1 and
cleanup with Florisil cartridge [10]. Eluent was ethyl acetate/dichloromethane 2:1
[10]. Recoveries were of 48–91% and MLODs of 3.1–1,100 pg/g lipid weight
(lw) [10]. Stir bar sorptive extraction (SBSE)-thermal desorption (TDU)-gas chromatography (GC) method was employed for the determination of pyrethroid residues in tea. As the tea samples were solid, a preliminary extraction with methanol
was implemented, and then the samples of methanol extraction were extracted by stir
bar sorptive extraction (SBSE) method [52]. Recoveries were of 93–105% and
MLODs were not reported [52].
Analytical Methods for Determining Pyrethroid Insecticides in Environmental and. . .
35
magnetic microextraction (IL-DMME) was developed as novel and facile extraction
technique for determination of pyrethroids in honey samples [45]. The method
consists of a combination of dispersive liquid-liquid microextraction (DLLME)
and dispersive microsolid-phase extraction using an ionic liquid ([C 6 MIM]NTf 2 )
and no-modified magnetic nanoparticles (S-BaFe), respectively [45]. Pyrethroids
were firstly extracted by the ionic liquid, and then the no-modified magnetic
nanoparticle was used to retrieve the ionic liquid containing the pyrethroids. Finally,
pyrethroids were extracted from nanoparticles by sonication using acetonitrile as
solvents. Recoveries were of 87–92% with MLODs of 0.03–0.05 μg/L [45]. Magnetic nanoparticles (MNPs) exhibit high selectivity and, in small amounts, can
provide high recovery of analytes, even from large-volume samples. They also
allow easy, rapid isolation of analytes using an external magnetic field. A competitive enzyme-linked immunosorbent assay (ELISA) method was employed for the
determination of cypermethrin and permethrin in agricultural products (wine, fruit,
and vegetable). No further cleanup was needed. Matrix interferences were minimized by diluting with phosphate-buffered saline containing 40% methanol
[48]. Recoveries were 74–99% with MLODs of 5–10 μg/kg [48]. QuEChERS
method was employed for extraction of pyrethroid pesticide residue from rice
grain [49]. Extraction was performed using acetonitrile, MgSO4, and NaCl. Recoveries were of 87–117% and MLODs were of 1 μg/kg [49]. SPME was employed for
extraction of pyrethroids from cucumber and watermelon samples using highperformance liquid chromatography combined with post-column photochemically
induced fluorimetry derivatization and fluorescence detector (HPLC-PIF-FD)
[50]. The optimum SPME conditions were extraction time 30 min, stirring rate
1,100 rpm, extraction temperature 65
C, sample pH 3, soaking time 7 min, desorption time 5 min, and acetonitrile content 25%. Recoveries were of 91–100% and
MLODs 1.3–5 μg/kg [50]. Liquid-liquid extraction of pyrethroids (cypermethrin and
deltamethrin) from pasteurized milk was performed using acetonitrile as extraction
solvent with cleanup by precipitation at low temperature without additional stages
for removal of fat interferences [51]. Recoveries were of 93% for cypermethrin and
84% for deltamethrin with MLODs of 7.5 ng/L [51]. From human breast milk,
pyrethroids were extracted by sonication with hexan/dichloromethane 2:1 and
cleanup with Florisil cartridge [10]. Eluent was ethyl acetate/dichloromethane 2:1
[10]. Recoveries were of 48–91% and MLODs of 3.1–1,100 pg/g lipid weight
(lw) [10]. Stir bar sorptive extraction (SBSE)-thermal desorption (TDU)-gas chromatography (GC) method was employed for the determination of pyrethroid residues in tea. As the tea samples were solid, a preliminary extraction with methanol
was implemented, and then the samples of methanol extraction were extracted by stir
bar sorptive extraction (SBSE) method [52]. Recoveries were of 93–105% and
MLODs were not reported [52].
Analytical Methods for Determining Pyrethroid Insecticides in Environmental and. . .
35