Post-harvest HPLC determination of chlorfluazuron residues in pears treated with different programs.
The present study was conducted to monitor the level of chlorfluazuron residues in pear samples in order to assess the risk posed by the presence of such residues to the consumer. Chlorfluazuron was sprayed onto pear trees at the recommended dose rate at two different times at 30 and 21 days prior to harvesting in one treatment, at 21 and 14 days prior to harvesting in another treatment, and three times at 30, 21 and 14 days prior to harvesting in a third treatment. Chlorfluazuron residues were extracted with acetonitrile and partitioned into ethyl acetate. The residue determination was performed on an Apollo C(18) column using HPLC with a UV detection of 254 nm following the clean-up of the extract by open column chromatography with Florisil. The versatility of this method was evidenced by its good linearity (>0.995) in the concentration range between 0.2 and 10 microg/mL. The majority of the mean recoveries at two different fortification levels, 0.05 and 0.25 ppm, ranged from 84.9 +/- 3.2 to 94.3 +/- 10.6, and the repeatability (as the relative standard deviation) from three repetitive determinations of recovery was between 3.8 and 11%. The calculated limit of detection (LOD) was 0.008 ppm and the limit of quantitation was 0.03 ppm. Trace amounts of chlorfluazuron were detectable when it was applied onto the pear trees at two or three times prior to harvesting; however, the levels of chlorfluazuron were not quantified. The excellent sensitivity and selectivity of this method allowed for quantitation and identification at low levels with a run time of less than 12 min. Chlorfluazuron can be used safely to protect pears when sprayed two or three times at 14 days prior to harvesting.
Shim
Jae-Han
JH
Natural Products Chemistry Laboratory, Institute of Agricultural Science and Technology, College of Agriculture and Life Science, Chonnam National University, 300 Yong-Bong Dong, Buk-Ku, Gwangju 500-757, Republic of Korea. jhshim@chonnam.ac.kr
Abd El-Aty
A M
AM
Choi
Jeong-Heui
JH
Choi
Yong-Sun
YS
D002851:Chromatography, High Pressure Liquid / Q000379:methods*; D010573:Pesticide Residues / Q000032:analysis*; D010671:Phenylurea Compounds / Q000032:analysis*; D011725:Pyridines / Q000032:analysis*; D031989:Pyrus / Q000737:chemistry*; D012015:Reference Standards; D015203:Reproducibility of Results; D012680:Sensitivity and Specificity; D013056:Spectrophotometry, Ultraviolet
D010573:Pesticide Residues; D010671:Phenylurea Compounds; D011725:Pyridines; C057223:chlorfluazuron