PMID- 17631102 OWN - NLM STAT- PubMed-not-MEDLINE DCOM- 20070907 LR - 20070716 IS - 1873-4324 (Electronic) IS - 0003-2670 (Linking) VI - 596 IP - 2 DP - 2007 Jul 23 TI - High-performance liquid chromatographic/ion-trap mass spectrometric speciation of aquatic mercury as its pyrrolidinedithiocarbamate complexes. PG - 242-50 AB - Mercury-pyrrolidinedithiocarbamate complexes are first time used for speciation of aquatic mercury with high-performance liquid chromatographic/ion trap-mass spectrometric method utilizing atmospheric pressure chemical ionization (APCI). The separation of the four mercury species was achieved in less than 5 min with a linear gradient profile of aqueous methanol from 70 up to 100% (v/v) in 4th min, isocratic elution at 100% up to 5th min and followed by a negative gradient to 70% in 6th min. The best separation was achieved on a reverse phase Zorbax Eclipse XDB C18 column (50 mm x 2.1 mm i.d., 1.8 microm particle size). The on-column limits of detection (injection volume 1 microL) were 370 pg for methylmercury (MeHg+), 280 pg for ethylmercury (EtHg+), 250 pg for phenylmercury (PhHg+) and 90 pg for inorganic mercury (Hg2+) when the data were collected in selective ion monitoring (SIM) mode. A method of isolation and preconcentration of the mercury species using a "home-made" C18 solid phase extraction (SPE) microcolumns was developed to enhance sensitivity of the method. The preconcentration factor as much as 2500 was achieved with on-column complex formation of mercury-pyrrolidinedithiocarbamate. Methanol (100%) was chosen for elution of preconcentrated mercury species. The method was applied for the determination of mercury species in river water samples. FAU - Houserova, Pavlina AU - Houserova P AD - Department of Chemistry and Biochemistry, Mendel University of Agriculture and Forestry, Zemedelska 1, Brno, CZ 613 00, Czech Republic. FAU - Matejicek, David AU - Matejicek D FAU - Kuban, Vlastimil AU - Kuban V LA - eng PT - Journal Article DEP - 20070616 PL - Netherlands TA - Anal Chim Acta JT - Analytica chimica acta JID - 0370534 EDAT- 2007/07/17 09:00 MHDA- 2007/07/17 09:01 CRDT- 2007/07/17 09:00 PHST- 2007/04/05 00:00 [received] PHST- 2007/06/06 00:00 [revised] PHST- 2007/06/10 00:00 [accepted] PHST- 2007/07/17 09:00 [pubmed] PHST- 2007/07/17 09:01 [medline] PHST- 2007/07/17 09:00 [entrez] AID - S0003-2670(07)01049-5 [pii] AID - 10.1016/j.aca.2007.06.020 [doi] PST - ppublish SO - Anal Chim Acta. 2007 Jul 23;596(2):242-50. doi: 10.1016/j.aca.2007.06.020. Epub 2007 Jun 16.