Organolead compounds mass spectrometry

Heisterkamp, M., DeSmaele, T., Candelone, J.E, Moens, L., Dams, R. and Adam, F.C. (1997) Inductively coupled plasma mass spectrometry hyphenated to capillary gas chromatography as a detection system for the speciation of organolead compounds in environmental waters./. Anal. At. Spectrom., 12, 1077-1081. 

Investigations of lead speciation in various environmental samples have relied upon gas and liquid chromatographic separations coupled to mass spectrometric and atomic absorption spectrometric detectors. The combination of atomic absorption spectrometry with gas chromatography (GC-AAS) has proved to be the most widely applied technique. Sample types have included air, surface water, air particulates, sediments, grass, and clinical materials such as blood. A review of speciation analyses of organolead compounds by GC-AAS, with emphasis on environmental materials, was published (Lobinski et al., 1994). 

Figure 7 Liquid chromatography inductively coupled plasma mass spectrometry (LC-ICP-MS) chromatogram of a standard mixture of organolead and inorganic lead compounds (Pb2+, TML, and TEL) using reversed-phase HPLC. Mobile phase, 0.1 M ammonium acetate, and 0.1 M acetic acid at pH 4.6, 30% ethanol. Flow rate 1 mL/min. (From Ref. 26.)...

Atomic absorption spectrometry (AAS) was established as the most popular gas chromatography (GC) detection technique for lead speciation analysis in the first years of speciation studies. The increase of the residence time of the species in the flame using a ceramic tube inside the flame and, later, the use of electrically heated tubes, made out of graphite or quartz where electrothermal atomization was achieved, provided lower detection limits but still not sufficiently low. Later, the boom of plasma detectors, mainly microwave induced plasma atomic emission (MIP-AES) and, above all, inductively coupled plasma atomic emission and mass spectrometry (ICP-AES and ICP-MS, respectively) allowed the sensitivity requirements for reliable organolead speciation analysis in environmental and biological samples (typically subfemtogram levels) to be achieved. These sensitivity requirements makes speciation analysis of organolead compounds by molecular detection techniques such as electrospray mass spectrometry (ES-MS) a very difficult task and, therefore, the number of applications in the literature is very limited. 

Radzuik et al have described a gas chromatographic-atomic absorption method using furnace atomization for the determination of alkyllead compounds in air. Gas chromatography-mass spectrometry was used to identify the separated organolead compounds. In this method, described below, the alkyl lead compounds are condensed from a 70-1 air sample in a series of four traps at - 72°C, separated by gas chromatography and determined by atomic absorption spectrometry with electrothermal atomization. 

Heisterkamp M. and Adams F. C. (2001) Gas chromatography-induc-tively coupled plasma-time-of-flight mass spectrometry for the speciation analysis of organolead compounds in environmental water samples, Frese-nius J. Anal. Chem. 370 597-605. 

Leal-Granadillo, I. A., Garcfa Alonso, J. I., and Sanz-Medel, A. (2000) Determination of the speciation of organolead compounds in airborne particulate matter by gas chromatography-inductively coupled plasma mass spectrometry. Anal. Chim. Acta, 432, 21-9. 

---