Pesticide Residue Research Group, Faculty of Experimental Sciences, University of Almeria, 04071-Almera, Spain.
J Agric Food Chem. 2010 Mar 10;58(5):2818-23. doi: 10.1021/jf904465s.
This paper describes the application of liquid chromatography time-of-flight mass spectrometry (LC/TOF-MS), with electrospray ionization, for residue analysis of forchlorfenuron in tomato, zucchini and watermelon. The assessed method includes a sample preparation step based on the buffered QuEChERS approach. The TOF-MS fragmentation pattern of forchlorfenuron was studied at different fragmention voltages in the range of 120-270 V. Analyses were carried out under full-scan conditions by using the extracted ion chromatogram (XIC) of the m/z 248 ion with a 0.2 Da window. The linearity of the analytical response across the studied range of concentrations (10-500 microg/kg) was excellent, obtaining correlation coefficients higher than 0.999, and relative standard deviations of the response factors lower than 14%, for the 15 linear calibration curves of forchlorfenuron evaluated along the complete validation study. No significant matrix effects were observed. The signal-to-noise ratios obtained for the 10 microg/kg forchlorfenuron in matrix matched standards were >70 for all three matrices. Recovery studies were carried out on spiked tomato, zucchini and watermelon blank samples, at three concentration levels (10, 50, and 200 microg/kg) performing five replicates at each level. Forchlorfenuron mean recoveries ranged between 80% and 87% in watermelon and zucchini, and between 65% and 71% in tomato, obtaining in all cases relative standard deviation values lower than 10%. The method readily achieved a lowest validated level of 10 microg/kg, which was fit-for-purpose in residue monitoring applications.
本文描述了液相色谱飞行时间质谱(LC/TOF-MS)在经电喷雾电离后,用于分析番茄、南瓜和西瓜中氯氟脲残留量的应用。评估方法包括基于缓冲 QuEChERS 方法的样品制备步骤。在 120-270 V 的范围内,研究了氯氟脲在不同碎片电压下的 TOF-MS 碎片模式。在全扫描条件下,使用 m/z 248 离子的提取离子色谱图(XIC),以 0.2 Da 的窗口进行分析。在所研究的浓度范围内(10-500μg/kg),分析响应的线性关系非常好,获得的相关系数均高于 0.999,15 条氯氟脲线性校准曲线的响应因子相对标准偏差均低于 14%,这是在整个验证研究中评估的。未观察到明显的基质效应。对于基质匹配标准中浓度为 10μg/kg 的氯氟脲,所有三种基质的信噪比均大于 70。在三个浓度水平(10、50 和 200μg/kg)下,对添加氯氟脲的番茄、南瓜和西瓜空白样品进行了回收率研究,每个水平重复五次。氯氟脲在西瓜和南瓜中的平均回收率在 80%至 87%之间,在番茄中的回收率在 65%至 71%之间,在所有情况下,相对标准偏差值均低于 10%。该方法很容易达到 10μg/kg 的最低验证水平,适用于残留监测应用。