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热脱附气相色谱-质谱法测定空气中的二氯二苯三氯乙烷。

Dichlorodiphenyltrichloroethane determination in air by thermal desorption gas chromatography-mass spectrometry.

机构信息

US Naval Medical Research Center, Silver Spring, MD 20910, USA.

出版信息

Pest Manag Sci. 2012 Oct;68(10):1360-7. doi: 10.1002/ps.3313. Epub 2012 Jun 6.

Abstract

BACKGROUND

Current quantitative methods for airborne dichlorodiphenyltrichloroethane (DDT) require collection and extraction times of ≥ 12 h. The aim of this study was to develop a method for quantifying airborne DDT with a short (<4 h) collection and analysis time.

RESULTS

Precision [relative standard deviation (RSD)] for each calibration point (0.8-9.0), linearity (R(2) = 0.99) and apparent recovery (R' = 96.5%) were determined from thermal desorption (TD) gas chromatography-mass spectrometry (GC-MS) analyses of Tenax-TA-packed sampling tubes spiked with 1-250 ng of DDT. Recovery of (13) C-labeled 4,4'-DDT from tubes spiked before and after air sampling was 97.3 and 90.3% respectively. DDT was detected and quantified in 1-3 L samples of air collected during 10-180 min sampling events. A significant difference was observed in DDT air concentration between 28 and 33 °C during microchamber studies.

CONCLUSIONS

The results demonstrate that the TD GC-MS method developed in this study is precise, reproducible and linear over the span of 1-250 ng of DDT spiked onto TD tubes. By avoiding dilution of the sample, the method described allows the measurement of DDT vapor concentrations during short sampling periods (10-180 min) relevant to mosquito behavior studies.

摘要

背景

目前空气中滴滴涕(DDT)的定量方法需要采集和提取时间≥12 小时。本研究的目的是开发一种可在短于 4 小时的采集和分析时间内定量空气中 DDT 的方法。

结果

通过对 Tenax-TA 填充采样管进行热解吸(TD)气相色谱-质谱(GC-MS)分析,确定了每个校准点(0.8-9.0)的精密度(相对标准偏差(RSD))、线性(R²=0.99)和表观回收率(R'=96.5%)。在空气采样前后对装有(13)C 标记的 4,4'-DDT 的采样管进行回收,分别为 97.3%和 90.3%。在 10-180 分钟的采样过程中,在 1-3 L 空气中采集到的空气样品中检测到并定量了 DDT。在微室研究中,在 28 和 33°C 之间观察到 DDT 空气浓度有显著差异。

结论

研究结果表明,本研究中开发的 TD-GC-MS 方法在 1-250 ng TD 管上添加 DDT 的范围内具有较高的精密度、重现性和线性。通过避免对样品进行稀释,所描述的方法允许在与蚊子行为研究相关的短采样时间(10-180 分钟)内测量 DDT 蒸气浓度。

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