Fang Fu, Hong Chia-Swee, Chu Shaogang, Kou Wenpeng, Bucciferro Anthony
Department of Environmental Health and Toxicology, School of Public Health, State University of New York at Albany, Albany, NY 12201-0509, USA.
J Chromatogr A. 2003 Dec 22;1021(1-2):157-64. doi: 10.1016/j.chroma.2003.08.069.
A headspace solid-phase microextraction (SPME) and gas chromatography-mass spectrometry (GC-MS) method has been reevaluated for the determination of methyl tert-butyl ether (MTBE) in water. Factors affecting method performance were examined. The internal standard, deuterated MTBE, is necessary because it allows normalization of the calibration since the deuterated MTBE and MTBE experience the same extraction efficiency. The method detection limit was 6.6 ng/l, with a linear range up to 160 microg/l. SPME extraction efficiency and detection sensitivity for MTBE decreased in the presence of gasoline matrix. However, reliable measurement of MTBE was possible in the background matrix concentration of 0.97 mg/l gasoline using deuterated internal standard. Reproducibility was 4.5% at the spiking level of 47 ng/l. The average recoveries of MTBE in spiked fountain water, tap water, and snow at 60 ng/l and in spiked rainwater at 580 ng/l ranged from 101 to 105%. The method was successfully applied to the analysis of trace levels of MTBE in various water samples, including rain and snow samples collected in Albany, NY, USA.
已对一种顶空固相微萃取（SPME）和气相色谱 - 质谱联用（GC - MS）方法进行重新评估，用于测定水中的甲基叔丁基醚（MTBE）。研究了影响方法性能的因素。内标物氘代MTBE是必需的，因为它能实现校准归一化，因为氘代MTBE和MTBE具有相同的萃取效率。方法检测限为6.6 ng/l，线性范围高达160 μg/l。在汽油基质存在的情况下，MTBE的SPME萃取效率和检测灵敏度会降低。然而，使用氘代内标物，在汽油背景基质浓度为0.97 mg/l时能够可靠地测量MTBE。在加标水平为47 ng/l时，重现性为4.5%。在加标浓度为60 ng/l的饮用泉水、自来水中以及加标浓度为580 ng/l的雨水中，MTBE的平均回收率在101%至105%之间。该方法成功应用于分析各种水样中的痕量MTBE，包括在美国纽约州奥尔巴尼采集的雨和雪样本。
