Hardy Emilie M, Duca Radu C, Salquebre Guillaume, Appenzeller Brice M R
Laboratory of Analytical Human Biomonitoring, Centre de Recherche Public de la Santé (CRP-Santé), 162A Avenue de la Faïencerie, L-1511 Luxembourg, Luxembourg.
Laboratory of Analytical Human Biomonitoring, Centre de Recherche Public de la Santé (CRP-Santé), 162A Avenue de la Faïencerie, L-1511 Luxembourg, Luxembourg.
Forensic Sci Int. 2015 Apr;249:6-19. doi: 10.1016/j.forsciint.2014.12.003. Epub 2014 Dec 13.
Urine being currently the most classically used matrix for the assessment of human exposure to pesticides, a growing interest is yet observed in hair analysis for the detection of organic pollutants. The aim of the present work was to develop and to validate multi-residue analytical methods, as similar as possible, in order to determine pesticides and their metabolites in these two biological matrices despite their different nature. The list of parent compounds and their metabolites investigated here consisted of 56 compounds, including organochlorines, organophosphates, pyrethroids, carbamates, other pesticides and polychlorinated biphenyls (PCBs). Two different approaches were necessary for the analysis of non-polar compounds (mainly parents) on one hand and polar analytes (mainly metabolites) on the other hand. In the final procedure, extraction from hair was carried out with acetonitrile/water after sample decontamination and pulverization. Extract was split into two fractions, which were analyzed directly with solid phase microextraction (SPME) injection for non-polar compounds and after derivatization with liquid injection for polar compounds. In urine, non-polar compounds were analyzed directly using SPME. Polar compounds were analyzed after acidic hydrolysis, liquid-liquid extraction with acetonitrile-cyclohexane-ethyl acetate, derivatization and liquid injection. Analysis was performed with gas chromatography tandem mass spectrometry operating in negative chemical ionization (GC-MS/MS-NCI) for all the compounds (non-polar and polar) in the two matrices. In hair, limits of quantification (LOQ) ranged from 0.02 pg/mg for trifluralin to 5.5 pg/mg for diethylphosphate. In urine, LOQ ranged from 0.4 pg/mL for α-endosulfan to 4 ng/mL for dimethyldithiophosphate. The analysis of samples supplemented with standards and samples collected from an animal previously submitted to chronic exposure to pesticides confirmed that all the compounds were analyzable in both hair and urine. In addition, the levels of sensitivity reached with these methods were quite satisfactory with regard to previously published studies, and also considering the number of compounds investigated.
尿液是目前评估人类接触农药时最经典使用的基质，但现在人们对通过头发分析检测有机污染物的兴趣也在不断增加。本研究的目的是开发并验证尽可能相似的多残留分析方法，以便在这两种性质不同的生物基质中测定农药及其代谢物。此处研究的母体化合物及其代谢物列表包含56种化合物，包括有机氯、有机磷、拟除虫菊酯、氨基甲酸酯、其他农药和多氯联苯（PCBs）。一方面分析非极性化合物（主要是母体），另一方面分析极性分析物（主要是代谢物）需要两种不同的方法。在最终程序中，头发样品经去污和粉碎后用乙腈/水进行萃取。萃取物分为两部分，一部分直接用固相微萃取（SPME）进样分析非极性化合物，另一部分经衍生化后用液体进样分析极性化合物。在尿液中，非极性化合物直接用SPME分析。极性化合物经酸性水解、用乙腈 - 环己烷 - 乙酸乙酯进行液 - 液萃取、衍生化和液体进样后进行分析。两种基质中的所有化合物（非极性和极性）均采用负化学电离模式运行的气相色谱串联质谱（GC - MS/MS - NCI）进行分析。在头发中，定量限（LOQ）范围从氟乐灵的0.02 pg/mg到磷酸二乙酯的5.5 pg/mg。在尿液中，LOQ范围从α - 硫丹的0.4 pg/mL到二甲基二硫代磷酸酯的4 ng/mL。对添加标准品的样品以及从先前长期接触农药的动物采集的样品进行分析，证实所有化合物在头发和尿液中均可分析。此外，就先前发表的研究以及所研究化合物的数量而言，这些方法达到的灵敏度水平相当令人满意。
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