Al Mahmud M N U, Rahman Musfiqur, Na Tae-Woong, Park Jong-Hyouk, Yang Angel, Park Ki Hun, Abd El-Aty A M, Nahar Nilufar, Shim Jae-Han
Natural Products Chemistry Laboratory, Biotechnology Research Institute, Chonnam National University, Buk-gu Gwangju, Republic of Korea.
Biomed Chromatogr. 2013 Feb;27(2):156-63. doi: 10.1002/bmc.2763. Epub 2012 Jun 25.
The objective of this work was to establish a simple extraction method for the residual analysis of pyraclofos and tebufenpyrad in Perilla leaves. A QuEChERS (quick, easy, cheap, effective, rugged and safe) method was used for extraction using ethyl acetate as an extraction solvent, and cleanup was carried out using dispersive solid-phase extraction technique. The samples were analyzed using gas chromatography with nitrogen phosphorous detector and confirmed by gas chromatography-mass spectrometry. The linearity was excellent (r(2) = 1.0) in matrix-matched calibration for both pesticides. The recoveries at two fortification levels were 80.76-95.38% with relative standard deviation lower than 5%. The limits of detection and limits of quantification were 0.01 and 0.033 mg/kg for both pesticides, respectively. The results revealed that the dissipation pattern of pyraclofos and tebufenpyrad followed first-order kinetics. The pyraclofos and tebufenpyrad residues declined to a level below the maximum residue limits within 14 day between the last application and harvesting. We suggest that pyraclofos and tebufenpyrad could be used efficiently on perilla leaves under the recommended dosage conditions.
本研究的目的是建立一种简单的紫苏叶中吡唑磷和联苯肼酯残留分析的提取方法。采用QuEChERS（快速、简便、廉价、有效、耐用且安全）方法，以乙酸乙酯作为提取溶剂进行提取，并采用分散固相萃取技术进行净化。使用配有氮磷检测器的气相色谱仪对样品进行分析，并通过气相色谱 - 质谱联用仪进行确证。两种农药在基质匹配校准中的线性关系良好（r(2) = 1.0）。两个加标水平下的回收率为80.76 - 95.38%，相对标准偏差低于5%。两种农药的检出限和定量限分别为0.01和0.033 mg/kg。结果表明，吡唑磷和联苯肼酯的消解模式符合一级动力学。在最后一次施药和收获之间的14天内，吡唑磷和联苯肼酯残留量降至最大残留限量以下。我们建议在推荐剂量条件下，吡唑磷和联苯肼酯可在紫苏叶上有效使用。
