Supplementary data on rapid sample clean-up procedure of aminophosphonates for LC/MS analysis

Abstract

Minimising matrix effects through high sample purity is of major importance for LC/MS analysis. Here we provide supplementary data and protocols related to the article “Rapid sample clean-up procedure of aminophosphonates for LC/MS analysis” (revised article submitted to Talanta) [1]. It is demonstrated that the tested phosphonates iminodi(methylenephosphonic acid) (IDMP), hydroxyethelidene(diphosphonic acid) (HEDP), aminotris(methylenephosphonic acid) (ATMP), ethylenediaminetetra(methyloenephosphonic acid) (EDTMP) and diethylenetriaminepenta(methylenephosphonic acid) (DTPMP) dissolved in tap water are not detectable by LC/MS without sample clean-up. Only the smallest aminophosphonate amino(methylenephosphonic acid) (AMPA) was detectable but the recovery is decreased drastically.The optimised sample clean-up with cation exchange resin (CER) Dowex 50WX8 is described in detail and illustrated. The protocol is provided. The influence of the incubation time, addition of different ammonium acetate concentrations, different samples pHs and different water qualities is demonstrated and preferred clean-up conditions are recommended. Calibration results of all tested aminophosphonates are validated regarding limit of detection, limit of quantification, lower limit of quantification, absolute and relative process standard deviation. A final recommendation for the best clean-up condition for all six tested aminophosphonates is provided. • AMPA analysis without derivatisation is possible with optimised clean-up procedure • Clean-up procedure is combinable with derivatisation method of [2] • Procedure is simple, rapid and highly reproducible

Keywords

• Phosphonates
• LC/MS analysis
• Cation Exchange Resin
• Clean-up