Lambropoulou D A, Sakkas V A, Albanis T A
Department of Chemistry, University of Ioannina, Greece.
Anal Bioanal Chem. 2002 Nov;374(5):932-41. doi: 10.1007/s00216-002-1549-7. Epub 2002 Oct 11.
Solid-phase microextraction (SPME) has been optimized and applied to the determination of the organophosphorus insecticides diazinon, dichlofenthion, parathion methyl, malathion, fenitrothion, fenthion, parathion ethyl, bromophos methyl, bromophos ethyl, and ethion in natural waters. Four types of SPME fiber coated with different stationary phases (PDMS, PA, PDMS-DVB, and CW-DVB) were used to examine their extraction efficiencies for the compounds tested. Conditions that might affect the SPME procedure, such as extraction time and salt content, were investigated to determine the analytical performance of these fiber coatings for organophosphorus insecticides. The optimized procedure was applied to natural waters - tap, sea, river, and lake water - spiked in the concentration range 0.5 to 50 micro g L(-1) to obtain the analytical characteristics. Recoveries were relatively high - >80% for all types of aqueous sample matrix - and the calibration plots were reproducible and linear (R(2)>0.982) for all analytes with all the fibers tested. The limits of detection ranged from 2 to 90 ng L(-1), depending on the detector and the compound investigated, with relative standard deviations in the range 3-15% at all the concentration levels tested. The SPME partition coefficients (K(f)) of the organophosphorus insecticides were calculated experimentally for all the polymer coatings. The effect of organic matter such as humic acids on extraction efficiency was also studied. The analytical performance of the SPME procedure using all the fibers in the tested natural waters proved effective for the compounds.
固相微萃取（SPME）已得到优化，并应用于天然水中有机磷杀虫剂二嗪农、毒虫畏、甲基对硫磷、马拉硫磷、杀螟硫磷、倍硫磷、对硫磷、甲基溴硫磷、乙基溴硫磷和乙硫磷的测定。使用四种涂覆不同固定相（聚二甲基硅氧烷（PDMS）、聚丙烯酸酯（PA）、聚二甲基硅氧烷-二乙烯基苯（PDMS-DVB）和碳分子筛-二乙烯基苯（CW-DVB））的SPME纤维来检测它们对所测试化合物的萃取效率。研究了可能影响SPME程序的条件，如萃取时间和盐含量，以确定这些纤维涂层对有机磷杀虫剂的分析性能。将优化后的程序应用于添加了浓度范围为0.5至50μg L⁻¹的自来水、海水、河水和湖水等天然水，以获得分析特性。回收率相对较高——所有类型的水样基质回收率均>80%，并且对于所有测试纤维的所有分析物，校准曲线均可重现且呈线性（R²>0.982）。检测限范围为2至90 ng L⁻¹，这取决于检测器和所研究的化合物，在所有测试浓度水平下相对标准偏差范围为3 - 15%。通过实验计算了所有聚合物涂层的有机磷杀虫剂的SPME分配系数（Kf）。还研究了腐殖酸等有机物对萃取效率的影响。在测试的天然水中使用所有纤维的SPME程序的分析性能证明对这些化合物有效。
