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Simultaneous determination of pyrethrolds from pesticide residues in porcine muscle and pasteurized milk using GC

机译:气相色谱法同时测定猪肌肉和巴氏消毒乳中农药残留中的拟除虫菊酯

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The principal goal of this work was to develop an efficient method for the simultaneous determination of four pyrethroid (PYR) insecticides, cyfluthrin, cyhalothrin, cypermethrin, and deltamethrin, in porcine muscle and pasteurized milk using liquid-liquid extraction (LLE). Sample extraction was carried out with and without additional column cleanup procedures, and the final determination was made using GC with electron-capture detector (ECD). The pesticide identity was confirmed using GC-MS in the SIM mode. Since there were minor differences between the extraction procedures, extraction without the additional cleanup procedure was used throughout the work. The method was validated by fortifying blank samples with half, two, and four times the maximum residue limit (MRL) of each PYR. The average recoveries (n = 6) ranged from 83.5 to 99.2% and 82.9 to 109% in porcine muscle and pasteurized milk, respectively. The repeatability of measurements expressed as RSDs, was in the range of 1.7-11.9 and 1.5-10.3% in porcine muscle and pasteurized milk, respectively. The LODs ranged from 3.3 to 9 and 3 to 8.1 ppm, whereas the LOQs ranged from 10 to 27.4 and 9 to 24.6 ppm, in porcine muscle and pasteurized milk, respectively. The applicability of the method was demonstrated by analyzing real samples collected from major cities in the Republic of Korea. No residues of the selected pesticides were detected in any of the samples.
机译:这项工作的主要目标是开发一种有效的方法,使用液-液萃取(LLE)同时测定猪肌肉和巴氏灭菌牛奶中的四种拟除虫菊酯(PYR)杀虫剂,氟氟氰菊酯,氟氯氰菊酯,氯氰菊酯和溴氰菊酯。在有和没有其他柱净化程序的情况下进行样品萃取,最后的测定是使用带电子捕获检测器(ECD)的GC进行的。使用SIM模式的GC-MS确认农药身份。由于提取程序之间的差异很小,因此在整个工作过程中都使用了没有额外清理程序的提取程序。通过用每个PYR的最大残留限量(MRL)的一半,两倍和四倍来加强空白样品,从而验证了该方法的有效性。猪肌肉和巴氏灭菌牛奶的平均回收率(n = 6)分别为83.5至99.2%和82.9至109%。在猪肌肉和巴氏杀菌牛奶中,以RSD表示的测量的重复性分别在1.7-11.9和1.5-10.3%的范围内。在猪肌肉和巴氏灭菌牛奶中,LOD的范围分别为3.3至9 ppm和3至8.1 ppm,而LOQ则为10至27.4 ppm和9至24.6 ppm。通过分析从大韩民国主要城市收集的真实样本,证明了该方法的适用性。在任何样品中均未检测到所选农药的残留。

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