A LC/APCI-MS/MS method for analysis of imidacloprid in soils, in plants, and in pollens
A LC/APCI-MS/MS method for analysis of imidacloprid in soils, in plants, and in pollens
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DOI：
10.1021/ac020600b
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发表时间：
2003-05-01
影响因子：
7.4
通讯作者：
Bengsch, ER
中科院分区：
文献类型：
--
作者：
Bonmatin, JM;Moineau, I;Bengsch, ER
使用最多的内吸性杀虫剂-吡虫啉，在每只蜜蜂纳克或每公斤微克的水平上，被怀疑对蜜蜂有有害影响。然而，缺乏检测如此低水平的吡虫啉及其代谢物的方法。建立了高效液相色谱-串联质谱法（APCI-MS/MS）测定土壤、植物（叶和花）和花粉中微量吡虫啉的方法。根据质量保证标准、药物非临床研究质量管理规范和针对禁用物质设计的指令96/23/EC的标准进行提取、分离和检测。在土壤、植物和花粉中，施用的线性范围为0.5-20 μ g/kg吡虫啉，1 μ g/kg时的相对标准偏差为2.9%。检测限和定量限分别为LOD = 0.1 μ g/kg和LOQ = 1 μ g/kg。这项研究第一次使我们能够跟踪吡虫啉在环境中的命运。当处理时，向日葵和玉米的花含有类似于10 μ g/kg的吡虫啉的平均值。Ibis解释说，这些作物的花粉受到污染的程度为每公斤几微克，这表明可能对蜜蜂产生有害影响。
Imidacloprid, the most used systemic insecticide, is suspected of having harmful effects on honeybees at nanogram per bee or at microgram per kilogram levels. However, there is a lack of methodology to detect imidacloprid and its metabolites at such low levels. We developed a method for the determination of low amounts of imidacloprid in soils, plants (leaves and flowers), and pollens by using HPLC coupled to tandem mass spectrometry (APCI-MS/MS). Extraction, separation, and detection were performed according to quality assurance criteria, to Good laboratory Practice, and to criteria from the directive 96/23/EC, which is designed for banned substances. The linear range of application is 0.5-20 mug/kg imidacloprid in soils, in plants, and in pollens, with a relative standard deviation of 2.9% at 1 mug/kg. The limits of detection and of quantification are LOD = 0.1 mug/kg and LOQ = 1 mug/kg, respectively. For the first time, this study permitted us to follow the fate of imidacloprid in the environment. When treated, flowers of sunflower and maize contain average values of similar to10 mug/kg imidacloprid. Ibis explains that pollens from these crops are contaminated at levels of a few micrograms per kilogram, suggesting probable deleterious effects on honeybees.