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Human Tracers as Surrogates for Potential Septic Contamination of Aquifers:Development and Test of an HPLC-UV Technique

机译:人类示踪剂作为潜在的含水层败血症的替代物:HPLC-UV技术的开发和测试

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There are numerous cases where ground waters have been found to be high in nitrate andrnattributed to either septic influence or agricultural practices. In many cases the nitrate datarnalone have been insufficient to differentiate between these causes for contamination. Correctivernmeasures in response to high nitrates vary depending upon the cause. With the advent of ultrasensitivernmethods for trace analysis for pharmaceuticals and personal care products (PPCPs) asrndemonstrated by the USGS (Kolpin et al, 2002), other analytical results could be used to shedrnlight on such situations. The Kolpin methods detect numerous compounds at the 1-50 part perrntrillion level. However they rely on LC-MS, expensive instrumentation that is not found inrnmost environmental labs. In contrast, HPLC systems are widely available in manyrncommercial and utility labs. Therefore the lab developed a sensitive HPLC/UV method for thernanalysis of 3 representative surrogate human tracers, caffeine, cotinine, and acetaminophen.rnThis HPLC method was targeted to achieve a reporting limit of 30 ppt (with a 10 ppt detectionrnlimit), sensitive enough to be useful in natural systems impacted by human activities.rnA 1000 milliliter (mL) sample aliquot is passed through a methanol and water conditionedrnWaters Oasis-HLB polymeric cartridge. After a sorbent wash step, the compounds are elutedrnfrom the cartridge with a small quantity of methanol followed by acidified methanol, andrnconcentrated further by evaporation of some of the solvent. A 10 mM Formate buffer is used tornbring the extract to volume. The extract is then analyzed by HPLC at two wavelengths (254rnand 280 nm) with conditions optimized to separate the compounds in a 15 minute run time.rnThis run time is short enough to allow analysis of large numbers of samples to establishrnpatterns of groundwater occurrence. The method was validated using a variety of standardrnprotocols to assess precision and accuracy (analysis of LFB, LFM, MRL checks). Asrnconfirmation of accuracy, selected samples are also analyzed for caffeine by a separate GCMSSPErnmethod that has a reporting limit of 5 ppt (MDL of 1 ppt).
机译:在许多情况下,发现地下水中的硝酸盐含量很高,并且归因于败血症影响或农业实践。在许多情况下,硝酸盐数据不足以区分这些污染原因。针对高硝酸盐的纠正措施因原因而异。随着USGS演示的用于药物和个人护理产品(PPCP)的痕量分析的超灵敏方法的出现(Kolpin等,2002),其他分析结果可用于阐明这种情况。 Kolpin方法可检测到1-50亿亿分之一水平的许多化合物。但是,它们依赖于LC-MS,这是在大多数环境实验室中都找不到的昂贵仪器。相反,HPLC系统可在许多商业和公用实验室中广泛使用。因此,实验室开发了一种灵敏的HPLC / UV方法来分析3种代表性替代人类示踪剂,咖啡因,可替宁和对乙酰氨基酚。该HPLC方法的目标是达到30 ppt的报告限(检测限为10 ppt),灵敏度足以在受人类活动影响的自然系统中有用。将1000毫升(mL)的等分试样通过甲醇和水调节过的Waters Oasis-HLB聚合物小柱。在吸附剂洗涤步骤之后,用少量甲醇从化合物盒中洗脱出化合物,然后将其酸化,然后通过蒸发一些溶剂进一步浓缩。使用10 mM的Formate缓冲液将提取物定容。然后通过HPLC在两个波长(254nm和280 nm)上对提取物进行分析,并优化了条件,以在15分钟的运行时间内分离出化合物。该运行时间足够短,可以分析大量样品以建立地下水发生模式。使用各种标准协议验证了该方法的准确性和准确性(LFB,LFM,MRL检查分析)。为确保准确性,还通过单独的GCMSSPErn方法对选定样品中的咖啡因进行了分析,该方法的报告限值为5 ppt(MDL为1 ppt)。

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