Kuhn Ramona, Bryant Isaac Mbir, Martienssen Marion
Brandenburg University of Technology Cottbus-Senftenberg, Institute of Environmental Technology, Chair of Biotechnology of Water Treatment, 03046 Cottbus, Germany.
MethodsX. 2020 May 23;7:100933. doi: 10.1016/j.mex.2020.100933. eCollection 2020.
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.•• [2]•.
通过高样品纯度来最小化基质效应对于液相色谱/质谱分析至关重要。在此,我们提供与文章《用于液相色谱/质谱分析的氨基膦酸盐快速样品净化程序》(已提交给《塔兰塔》杂志的修订文章)[1]相关的补充数据和实验方案。结果表明,溶解于自来水中的受试膦酸盐亚氨基二(亚甲基膦酸)(IDMP)、羟基亚乙基二膦酸(HEDP)、氨基三亚甲基膦酸(ATMP)、乙二胺四亚甲基膦酸(EDTMP)和二亚乙基三胺五亚甲基膦酸(DTPMP),若不进行样品净化,液相色谱/质谱无法检测到。只有最小的氨基膦酸盐氨基(亚甲基膦酸)(AMPA)可被检测到,但回收率急剧下降。详细描述并说明了使用阳离子交换树脂(CER)Dowex 50WX8进行的优化样品净化过程,并提供了实验方案。展示了孵育时间、不同醋酸铵浓度添加量、不同样品pH值和不同水质的影响,并推荐了优选的净化条件。针对所有受试氨基膦酸盐的检测限、定量限、定量下限、绝对和相对过程标准偏差,验证了校准结果。给出了针对所有六种受试氨基膦酸盐最佳净化条件的最终建议。•• [2]•.