Detection of hexamethonium‐perchlorate association complexes using NACE‐MS

Abstract

Perchlorate (ClO(4) (+)) and other chlorine oxide anions were observed to complex weakly with hexamethonium (1,6-bis-(trimethylammonium)-hexane) in both aqueous and polar nonaqueous solvents. The resultant positively charged complexes were resolved by NACE using 2-propanol/acetone electrolytes prior to mass spectrometric detection using an Agilent(3D)CE system coupled to a Bruker Esquire 3000+ quadrupole IT mass detector. Using electrokinetic injection, the method detection limit for perchlorate in nonaqueous media was 10 microg/L. The isotope patterns due to the presence of (35)Cl and (37)Cl in complex mass spectra allowed for unambiguous identification of perchlorate, chlorate (ClO(3) (+)), chlorite (ClO(2) (+)), and chloride (Cl(+)) in photoreaction samples.

Online Coupling of Capillary Electrophoresis with Direct Analysis in Real Time Mass Spectrometry

“…For generation of the new CE-DART-MS interface, it is important to introduce additional liquid at the outlet of the CE capillary to stabilize the electric current. The commercial Agilent sheath liquid tip (Palo Alto, CA, USA) − matched our thought with good quality. The tip was grounded without high voltage; therefore, no electrospray will be created.…”

Inorganic species analysis by CE – An overview for 2007–2008

“…However, dilution at the stage of sample preparation using microwave‐assisted extraction did not permit the determination of species other than bromide and iodide. Chlorine oxide anions were identified in photoreaction samples by CE‐ESI‐MS after formation of ion‐pair complexes with the cationic surfactant hexamethonium and their separation by NACE using 2‐propanol/acetone electrolytes 54. Quantification of various inorganic forms of nitrogen, including ammonium, in plant material was feasible by CE‐UV and the results were used to understand the uptake and assimilation of NO 2 55.…”

“…Alternatively, a commercial chiral capillary with zwitterionic coating was used to separate diastereomers of an Fe(III) chelate 106, the resolution being improved with increasing amounts of ACN in the BGE. Organic solvents may also be an attractive selection as separation medium well‐suited for a specific detection mode 54, 107, 108 or poorly soluble/stable analytes 109, 110. In a latter theoretical study by Kenndler et al , methanol and ACN, together with water, were solvents of the BGE in which the electrophoretic properties of the anions of boron cluster compounds were determined as a function of the ionic strength.…”