Del Valle P L, Nelson J O
Marine-Estuarine Environmental Sciences (MEES) Program, University of Maryland, College Park 20742.
Arch Environ Contam Toxicol. 1994 Oct;27(3):375-83. doi: 10.1007/BF00213174.
Four soil extraction methods were evaluated for the determination of atrazine and other s-triazines by ELISA and GC, using both field-treated and laboratory fortified samples. The most efficient recoveries for atrazine, simazine, and cyanazine from loam soil fortified at concentrations from 0.01 ppm to 1 ppm were obtained by mechanical wrist-action shaker (1 h) using methanol:water and solid phase extraction (SPE) cleanup (standard method). A handshaking extraction (1 min) with acetonitrile:water showed fairly good correlation with the standard extraction method and is suitable for field use with ELISA. Sonication using acetonitrile:water and SPE cleanup was the most efficient extraction method for the dealkylated metabolites (deisopropyl and deethyl atrazine) with recoveries higher than 60%. In general, supercritical fluid extraction (SFE) was as efficient as sonication and handshaking but was more variable. A guideline for validation of immunoassays and methods comparison is given. The sensitivity of the ELISA method was comparable to the GC and was both accurate and precise. Comparison of ELISA and GC determinations of 120 field soil samples and 40 laboratory spiked soil samples extracted with four different methods showed no false negatives or positives with excellent correlations and showed not significant differences (P > 0.05). An evaluation of the cost for GC and ELISA methods was also conducted.
采用现场处理样品和实验室加标样品,对四种土壤提取方法进行了评估,以通过酶联免疫吸附测定法(ELISA)和气相色谱法(GC)测定阿特拉津和其他均三嗪。对于添加浓度为0.01 ppm至1 ppm的壤土中的阿特拉津、西玛津和氰草津,使用甲醇:水通过机械手腕振荡器振荡(1小时)并采用固相萃取(SPE)净化(标准方法)可获得最高效的回收率。用乙腈:水进行手动振荡萃取(1分钟)与标准萃取方法显示出相当好的相关性,适用于现场ELISA检测。使用乙腈:水超声处理并结合SPE净化是提取去烷基化代谢物(去异丙基阿特拉津和去乙基阿特拉津)最有效的萃取方法,回收率高于60%。总体而言,超临界流体萃取(SFE)与超声处理和手动振荡萃取效率相当,但变异性更大。给出了免疫分析验证和方法比较的指南。ELISA方法的灵敏度与GC相当,且准确精密。对120个现场土壤样品和40个用四种不同方法萃取的实验室加标土壤样品进行ELISA和GC测定的比较,结果显示无假阴性或假阳性,相关性良好且无显著差异(P>0.05)。还对GC和ELISA方法的成本进行了评估。