Evaluation of superficially and fully porous particles for HILIC separation of lanthanide–polyaminocarboxylic species and simultaneous coupling to ESIMS and ICPMS

Abstract

Application of sustainable chromatographic strategies to reduce effluent volumes generated by HILIC separation of lanthanide–polyaminocarboxylic acid species.

Developing and downscaling a method by HILIC coupled simultaneously to ESIMS and ICPMS to determine the affinity of lanthanide chelating molecules using specific isotope dilution

“…HILIC separations of Ln (Er, Eu, Gd, and Nd) with strong chelating molecules such as DTPA and EDTA have been previously investigated 13,31 and our first tests in this work showed that the nat Sm/ nat Nd–DTPA complexes were more retained than the complexes containing NM and TPAEN molecules. Hence, our efforts were first focused on the screening of the selectivity of several columns to separate nat Sm and nat Nd complexes of NM and TPAEN.…”

“…The instrumental configuration of the simultaneous coupling of HILIC in conventional separation format to ESIMS and the ICPMS XSeriesII was previously developed in the laboratory. 13 By applying this setup, the outflow from the column was split to enter the ESIMS with a flow rate of 295 µL min −1 (98.3%) and 5 µL min −1 for the flow entering the ICPMS (1.7%). A make-up made of 2% HNO 3 w/w and containing 10 ppb of 209 Bi as internal standard was added to the flow entering the ICPMS, with a flow rate of 140 µL min −1 .…”

“…For all the chelating molecules, complexes of 1/1 stoichiometry were online observed in agreement with the literature, in which TPAEN complexes were characterized by spectroscopic techniques 11 and DTPA complexes using HILIC-ESIMS. 13,31 In this study, the HILIC conditions have been set up to separate new sets of Ln complexes formed with hydrophilic synthetic chelating molecules, thanks to an amide functionalized stationary phase. Regarding the studies of Ln species, numerous studies have reported the analysis of Gd-based contrast agents containing DTPA and linear/cyclic polyaminocarboxylic acid derivatives such as BT-DO3A, DOTA, BMA and BOPTA, by HILIC-ESIMS 20 and/or HILIC-ICPMS in blood plasma and urine samples, 21-23 waters [23][24][25][26][27][28][29] and plants.…”

“…To meet this goal, the strategy of this work was based on the simultaneous coupling of hydrophilic liquid chromatography (HILIC) to electrospray ionization mass spectrometry (ESIMS) and inductively coupled plasma mass spectrometry (ICPMS) previously set up in the laboratory. 13 This powerful approach allows, online and simultaneously, the structural, multi-elemental and isotopic characterization of chemical species coming from the chromatographic separation. Hence, the quantitative distribution of the elements among the complexes formed with the different chelating molecules (CMs) in a sample can be determined, allowing the selectivity and the affinity of the molecules for the elements to be reached, in a single analysis.…”

Fundamental to achieving fast separations with high efficiency: A review of chromatography with superficially porous particles

“…As discussed earlier, SPP-HILIC is powerful for analyzing polar compounds, which is superior to TPP-HILIC for fast separations. It has been reported that SPP-HILIC phases have been used in quantitatively determining S-nitrosoglutathione in human plasma (Tsikas et al, 2013), in neuroscience such as the major inhibitory and excitatory neurotransmitters, γ-aminobutyric acid and L-glutamic acid (Defaix et al, 2018), and betaines and other quaternary ammoniumrelated compounds in bee pollen (Ares et al, 2020), in cosmetics to detect harmful impurities (Wang & Zhou, 2016), in the food industry such as amino acids and other components in dietary supplements (Themelis et al, 2017), and in the nuclear industry such as detecting lanthanide-polyaminocarboxylic species (Blanchard et al, 2018). It was also reported that HILIC phase can beneficially combine as a second dimension with a chiral column for comprehensive 2D LC (Bäurer et al, 2020).…”