Group "Analytical Chemistry of Contaminants", Department of Analytical Chemistry, Almeria University, E-04071 Almeria, Spain.
Talanta. 2011 Jul 15;85(1):183-96. doi: 10.1016/j.talanta.2011.03.048. Epub 2011 Mar 31.
A new multiresidue method has been developed and validated for the simultaneous extraction of more than two hundred pesticides, including non-polar and polar pesticides (carbamates, organochlorine, organophosphorous, pyrethroids, herbicides and insecticides) in urine at trace levels by gas and ultra high pressure liquid chromatography coupled to ion trap and triple quadrupole mass spectrometry, respectively (GC-IT-MS/MS, UHPLC-QqQ-MS/MS). Non-polar and polar pesticides were simultaneously extracted from urine samples by a simple and fast solid phase extraction (SPE) procedure using C(18) cartridges as sorbent, and dichloromethane as elution solvent. Recovery was in the range of 60-120%. Precision values expressed as relative standard deviation (RSD) were lower than 25%. Identification and confirmation of the compounds were performed by the use of retention time windows, comparison of spectra (GC-amenable compounds) or the estimation of the ion ratio (LC-amenable compounds). For GC-amenable pesticides, limits of detection (LODs) ranged from 0.001 to 0.436 μg L(-1) and limits of quantification (LOQs) from 0.003 to 1.452 μg L(-1). For LC-amenable pesticides, LODs ranged from 0.003 to 1.048 μg L(-1) and LOQs ranged from 0.011 to 3.494 μg L(-1). Finally, the optimized method was applied to the analysis of fourteen real samples of infants from agricultural population. Some pesticides such as methoxyfenozide, tebufenozide, piperonyl butoxide and propoxur were found at concentrations ranged from 1.61 to 24.4 μg L(-1), whereas methiocarb sulfoxide was detected at trace levels in two samples.
已开发并验证了一种新的多残留方法，用于通过气相和超高压液相色谱分别与离子阱和三重四极杆质谱联用（GC-IT-MS/MS、UHPLC-QqQ-MS/MS），同时提取痕量水平尿液中的 200 多种农药，包括非极性和极性农药（氨基甲酸酯、有机氯、有机磷、拟除虫菊酯、除草剂和杀虫剂）。使用 C(18) 小柱作为吸附剂，二氯甲烷作为洗脱溶剂，通过简单快速的固相萃取（SPE）程序从尿液样品中同时提取非极性和极性农药。回收率在 60-120%之间。以相对标准偏差（RSD）表示的精密度值低于 25%。通过使用保留时间窗口、比较光谱（GC 可分析化合物）或估计离子比（LC 可分析化合物）来进行化合物的鉴定和确认。对于 GC 可分析的农药，检测限（LOD）范围为 0.001 至 0.436 μg/L，定量限（LOQ）范围为 0.003 至 1.452 μg/L。对于 LC 可分析的农药，LOD 范围为 0.003 至 1.048 μg/L，LOQ 范围为 0.011 至 3.494 μg/L。最后，优化后的方法应用于 14 份来自农业人群的婴儿的实际样本分析。在一些样本中发现了甲氧虫酰肼、噻嗪酮、增效醚和残杀威等农药，浓度范围为 1.61 至 24.4 μg/L，而在两个样本中检测到甲硫环磷亚砜的痕量水平。
