Tomkins B A, Griest W H
Organic Chemistry Section, Oak Ridge National Laboratory, Tennessee 37831-6120, USA.
Anal Chem. 1996 Aug 1;68(15):2533-40. doi: 10.1021/ac9601573.
A new solid-phase extraction procedure extracts N-nitrosodimethylamine (NDMA) at part-per-trillion (ng/L) concentrations from aqueous samples using a C18 (reversed-phase) membrane extraction disk layered over a recently introduced carbon-based extraction disk. The reversed-phase disk removes nonpolar water-insoluble neutrals and is set aside; the carbon-based disk is extracted with a small volume of dichloromethane. NDMA is quantified in the organic extract using a gas chromatograph equipped with both a short-path thermal desorber and a chemiluminescent nitrogen detector. The detection limit for the procedure, calculated using two statistically unbiased protocols, is 3 ng of NDMA/L; the analyte recovery is approximately 57%. A related procedure substitutes a standard automatic sampler for the short-path thermal desorber and is suitable for determining NDMA in heavily contaminated (> 300 ng of NDMA/L) aqueous samples. The detection limit for the procedure, calculated in the same manner as above, is 300 ng of NDMA/L, with an analyte recovery of approximately 64%. The detection limits and measured recovery values are comparable to those observed in earlier work, in which a conventional continuous overnight extraction with dichloromethane was used to remove NDMA from the aqueous samples. The newer procedures described herein offer a 50-fold savings in extraction time and a 100-fold reduction in dichloromethane consumed per sample while maintaining the wide range (3-4 orders of magnitude concentrations of NDMA) observed for the original procedures used in tandem. Authentic contaminated groundwaters are extracted using both the conventional and disk-based extraction procedures and analyzed; the observed NDMA concentrations are virtually identical over a target range spanning 100-10000 ng of NDMA/L.
一种新的固相萃取方法,使用覆盖在最近推出的碳基萃取盘上的C18(反相)膜萃取盘,从水样中以万亿分之一(ng/L)浓度萃取N-亚硝基二甲胺(NDMA)。反相盘去除非极性水不溶性中性物质后被搁置一旁;碳基盘用少量二氯甲烷萃取。使用配备短路径热解吸器和化学发光氮检测器的气相色谱仪对有机萃取物中的NDMA进行定量。使用两种无统计学偏差的方案计算得出,该方法的检测限为3 ng NDMA/L;分析物回收率约为57%。一种相关方法用标准自动进样器替代短路径热解吸器,适用于测定严重污染(>300 ng NDMA/L)水样中的NDMA。以与上述相同的方式计算得出,该方法的检测限为300 ng NDMA/L,分析物回收率约为64%。检测限和测得的回收率值与早期工作中观察到的值相当,早期工作中使用二氯甲烷进行传统的连续过夜萃取以从水样中去除NDMA。本文所述的新方法在萃取时间上节省了50倍,每个样品消耗的二氯甲烷减少了100倍,同时保持了串联使用的原始方法所观察到的宽范围(NDMA浓度为3 - 4个数量级)。使用传统和基于盘的萃取方法对真实受污染的地下水进行萃取并分析;在100 - 10000 ng NDMA/L的目标范围内观察到的NDMA浓度几乎相同。