Shim Jae-Han, Abd El-Aty A M, Choi Jeong-Heui, Choi Yong-Sun
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.
Biomed Chromatogr. 2007 Jul;21(7):695-700. doi: 10.1002/bmc.807.
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.
本研究旨在监测梨样品中氟啶脲残留水平,以评估此类残留对消费者造成的风险。在一种处理方式中,于收获前30天和21天分两次按照推荐剂量率向梨树上喷洒氟啶脲;在另一种处理方式中,于收获前21天和14天喷洒;在第三种处理方式中,于收获前30天、21天和14天分三次喷洒。用乙腈提取氟啶脲残留并分配至乙酸乙酯中。提取物经弗罗里硅土柱色谱净化后,在Apollo C(18)柱上使用高效液相色谱法(HPLC)并在254 nm波长处进行紫外检测来测定残留量。该方法在0.2至10 μg/mL浓度范围内具有良好的线性(>0.995),证明了其通用性。在0.05和0.25 ppm这两个不同加标水平下,大多数平均回收率在84.9±3.2至94.3±10.6之间,三次重复回收率测定的重复性(相对标准偏差)在3.8%至11%之间。计算得出的检测限(LOD)为0.008 ppm,定量限为0.03 ppm。在收获前向梨树上喷洒两次或三次氟啶脲时可检测到痕量的氟啶脲,但未对其含量进行定量。该方法出色的灵敏度和选择性使得能够在不到12分钟的运行时间内对低水平的氟啶脲进行定量和鉴定。在收获前14天向梨树上喷洒两次或三次氟啶脲时,可安全使用氟啶脲来保护梨树。