Instrumental Laboratory, Technological National Center of Canning Industry (CTC), Murcia, Spain.
J Environ Sci Health B. 2011;46(6):525-9. doi: 10.1080/03601234.2011.583873.
A method for the detection and quantification of 16 pesticides: flufenoxuron, fenoxycarb, dimethomorph, acetamiprid, imidacloprid, lufenuron, thiacloprid, thiabendazole, thiophanate-methyl, spinosad, fenbutatin oxide, methoxyfenozide, oxamyl, clothianidin, thiamethoxam and carbendazim has been developed based on high-performance liquid chromatography-mass spectrometry. Pesticide residues were extracted from the samples according to the QuEChERS method which stands for quick, essay, cheap, effective, rugged and safe. Homogenised analytical portions (10 g ± 0.1) of samples of peppers were spiked at two levels (10 and 100 μg kg⁻¹) with a small volume of an appropriate standard mixture solution containing each pesticide. Analyses were performed using electrospray ionization (ESI) and a MSD trap system. Chromatography separation was achieved using a ZORBAX SB-C18 3.5 μm particle size analytical column, 2.1 × 50 mm from Agilent, with gradient elution at a flow-rate of 0.4 mL/min with mobile phases: waters-0.1 % HCOOH-5 mM HCOONH₄ and MeOH-5 mM HCOONH₄. The method has been validated based on the SANCO European Guidelines. Under the optimized conditions the recoveries (n = 7) were in the range 70-110 % with satisfactory precision (CV ≤ 20 %). A linear dynamic range was obtained over a range of concentrations from 10 to 100 μg kg⁻¹ for each of the analytes, with correlation coefficients >0.997.
基于高效液相色谱-质谱法开发了一种检测和定量 16 种农药：氟虫脲、苯氧威、烯酰吗啉、乙虫腈、噻虫啉、灭蝇脲、噻虫嗪、噻菌灵、噻虫胺、多杀菌素、丁醚脲、甲氧虫酰肼、氧乐果、噻虫啉、氯虫苯甲酰胺、噻虫嗪和多菌灵的方法。根据 QuEChERS 方法从样品中提取农药残留，QuEChERS 代表快速、简单、廉价、有效、坚固和安全。将胡椒的均质分析部分（10 g ± 0.1）以小体积的适当标准混合溶液添加到两个水平（10 和 100 μg kg⁻¹），其中包含每种农药。使用电喷雾电离（ESI）和 MSD 阱系统进行分析。使用 ZORBAX SB-C18 3.5 μm 粒径分析柱，Agilent 公司的 2.1 × 50 mm，在流速为 0.4 mL/min 下进行梯度洗脱，流动相为：水-0.1 % HCOOH-5 mM HCOONH₄ 和 MeOH-5 mM HCOONH₄。该方法是根据 SANCO 欧洲准则进行验证的。在优化条件下，回收率（n = 7）在 70-110%范围内，精密度令人满意（CV ≤ 20%）。在 10 至 100 μg kg⁻¹的浓度范围内，每个分析物都获得了线性动态范围，相关系数>0.997。
