TY - JOUR
T1 - Simultaneous Determination of 69 Pesticide Residues in Coffee by Gas Chromatography-Mass Spectrometry
AU - Yang, Xin
AU - Wang, Jing
AU - Xu, D. C.
AU - Qiu, J. W.
AU - Ma, Ying
AU - Cui, J.
PY - 2011/6
Y1 - 2011/6
N2 - A method using gel permeation chromatography (GPC) combined with solid-phase extraction (SPE) cleanup followed by gas chromatography-mass spectrometry (GC-MS) has been established for quantitative determination of 69 pesticide residues in coffee. Based on an appraisal of the characteristics of GC-MS, validation experiments were conducted for 69 pesticides. In the method, 2.0 g samples were mixed with 5 ml water and 1 g sodium chloride and extracted with 5 ml of ethyl acetate by blender homogenization, centrifugation, and filtration. Evaporation was conducted and the sample was injected into a 250 mm × 10 mm S-X3 GPC column, with ethyl acetate-n-hexane (1:2 v/v) as the mobile phase at a flow rate of 3 ml/min. The 4-15 min fraction was collected for the SPE cleanup, which was Envi-Carb SPE cartridge coupled with NH 2-LC SPE cartridge with acetone-ethyl acetate (2:5 v/v) as the eluted solvent. The eluents were collected and then evaporated to dryness, which was redissolved in 0. 5 ml ethyl acetate for GC-MS analysis. For the 69 pesticides determined by GC-MS, the portions collected from GPC were concentrated to 0.5 ml and exchanged with 5 ml n-hexane. In the linear range of each pesticide, the correlation coefficient was R 2 ≥ 0.99. At the low, medium, and high fortification levels of 0. 05-1.0 mg/kg, recoveries fell within 60-120%. The relative standard deviation was between 1.3% and 22.3% for all 69 pesticides. The limits of detection for the method were 10 μg/kg to 150 μg/kg, depending on each pesticide.
AB - A method using gel permeation chromatography (GPC) combined with solid-phase extraction (SPE) cleanup followed by gas chromatography-mass spectrometry (GC-MS) has been established for quantitative determination of 69 pesticide residues in coffee. Based on an appraisal of the characteristics of GC-MS, validation experiments were conducted for 69 pesticides. In the method, 2.0 g samples were mixed with 5 ml water and 1 g sodium chloride and extracted with 5 ml of ethyl acetate by blender homogenization, centrifugation, and filtration. Evaporation was conducted and the sample was injected into a 250 mm × 10 mm S-X3 GPC column, with ethyl acetate-n-hexane (1:2 v/v) as the mobile phase at a flow rate of 3 ml/min. The 4-15 min fraction was collected for the SPE cleanup, which was Envi-Carb SPE cartridge coupled with NH 2-LC SPE cartridge with acetone-ethyl acetate (2:5 v/v) as the eluted solvent. The eluents were collected and then evaporated to dryness, which was redissolved in 0. 5 ml ethyl acetate for GC-MS analysis. For the 69 pesticides determined by GC-MS, the portions collected from GPC were concentrated to 0.5 ml and exchanged with 5 ml n-hexane. In the linear range of each pesticide, the correlation coefficient was R 2 ≥ 0.99. At the low, medium, and high fortification levels of 0. 05-1.0 mg/kg, recoveries fell within 60-120%. The relative standard deviation was between 1.3% and 22.3% for all 69 pesticides. The limits of detection for the method were 10 μg/kg to 150 μg/kg, depending on each pesticide.
KW - Coffee
KW - GC-MS
KW - GPC
KW - Multi-residue Analysis
KW - Pesticides
KW - SPE
UR - http://www.scopus.com/inward/record.url?scp=79955068673&partnerID=8YFLogxK
U2 - 10.1007/s12161-010-9155-3
DO - 10.1007/s12161-010-9155-3
M3 - Article
AN - SCOPUS:79955068673
SN - 1936-9751
VL - 4
SP - 186
EP - 195
JO - Food Analytical Methods
JF - Food Analytical Methods
IS - 2
ER -