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用于测定挥发性和非挥发性、极性和非极性N-亚硝基化合物的综合分析程序。

Comprehensive analytical procedures for the determination of volatile and non-volatile, polar and non-polar N-nitroso compounds.

作者信息

Fan T Y, Krull I S, Ross R D, Wolf M H, Fine D H

出版信息

IARC Sci Publ (1971). 1978(19):3-17.

PMID:680730
Abstract

The first comprehensive analytical procedures for the quantitative analysis of N-nitroso compounds are described. The scheme divides N-nitroso compounds into four major, overlapping categories: volatile (Class I), non-volatile, low polarity (Class II), non-volatile, non-ionic, high polarity (Class III) and non-volatile, ionic, high polarity (Class IV). Existing analytical techniques for each class of compound are integrated into an organized and logical sequence of analysis to allow all classes of compounds to be determined. TEA-GC is used for the volatile compounds and TEA-HPLC for the non-volatile. It is emphasized that the coincidence of retention time in either TEA-GC alone or TEA-HPLC alone cannot be taken as sufficient evidence for the identification of N-nitroso compounds, especially for samples from complex matrices. Independent techniques are required to confirm these results. The confirmatory techniques used frequently in our laboratory are: (1) spectroscopic analysis (IR, NMR, UV and MS), (2) formation and identification of derivatives, and (3) parallel TEA-GC/TEA-HPLC techniques. These procedures are now used at Thermo Electron for the comprehensive screening of environmental samples.

摘要

本文描述了用于N-亚硝基化合物定量分析的首个综合分析程序。该方案将N-亚硝基化合物分为四个主要的、相互重叠的类别:挥发性(I类)、非挥发性、低极性(II类)、非挥发性、非离子性、高极性(III类)和非挥发性、离子性、高极性(IV类)。将各类化合物现有的分析技术整合到一个有组织且符合逻辑的分析序列中,以便能够测定所有类别的化合物。气相色谱-热导分析仪(TEA-GC)用于挥发性化合物的分析,高效液相色谱-热导分析仪(TEA-HPLC)用于非挥发性化合物的分析。需要强调的是,仅凭TEA-GC或TEA-HPLC单独的保留时间一致,不能作为鉴定N-亚硝基化合物的充分证据,尤其是对于来自复杂基质的样品。需要采用独立技术来确认这些结果。我们实验室经常使用的确认技术有:(1)光谱分析(红外光谱、核磁共振、紫外光谱和质谱),(2)衍生物的形成与鉴定,以及(3)平行TEA-GC/TEA-HPLC技术。这些程序目前在赛默飞世尔科技公司用于环境样品的全面筛查。

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