Skip to Content
Merck
  • High-throughput automatic flow method for determination of trace concentrations of aluminum in dialysis concentrate solutions using salicylaldehyde picolinoylhydrazone as a turn-on fluorescent probe.

High-throughput automatic flow method for determination of trace concentrations of aluminum in dialysis concentrate solutions using salicylaldehyde picolinoylhydrazone as a turn-on fluorescent probe.

Talanta (2014-12-02)
Arnau Garau, Miquel Oliver, María Rosende, Manuel P Mánuel-Vez, Manuel Miró
ABSTRACT

A simple and expedient flow-based assembly capitalizing on programmable flow is herein proposed for reliable determination of trace level concentrations of aluminum as a potential contaminant in dialysis concentrate solutions without any prior sample clean-up/preconcentration procedure. Using salicylaldehyde picolinoylhydrazone in weakly acidic media as a turn-on fluorescent probe, the manifold is devised to handle three samples concurrently in stopped-flow reaction mode for simultaneous improvement of the analytical sensitivity and sample throughput. Analytical parameters influencing the sensitivity and repeatability of the assays, namely, probe concentration, reaction temperature and reaction time were investigated using a multivariate optimization protocol composed of a full factorial screening design followed by a Doehlert matrix model. The analysis of the Pareto chart and surface response revealed that the reaction time and amount of fluorescent probe were critical parameters for reliable assays of aluminum at the low ng mL(-1) level. Under the optimized chemical and physical variables, a detection limit of 1.1ngmL(-1) Al(III) at the 3s(blank) level, relative standard deviations better than 1.0%, a dynamic linear range of 5.0-80 ng mL(-1) and a sample throughput up to 25 h(-1) were obtained with no need for either sample preconcentration or the use of organized supramolecular systems. Demonstrated with the analysis of hemodialysis and peritoneal concentrate solutions, and dialysis waters, the flow-through method copes with the requirements of regulatory bodies (e.g., European Pharmacopeia) for quality control of aluminum in high salinity containing dialysis concentrates.

MATERIALS
Product Number
Brand
Product Description

Sigma-Aldrich
Acetic acid-12C2, 99.9 atom % 12C
Supelco
Acetic acid, analytical standard
Sigma-Aldrich
Ethyl 2-picolinate, 99%
Sigma-Aldrich
Acetic acid, ≥99.5%, FCC, FG
Sigma-Aldrich
Acetic acid, natural, ≥99.5%, FG
Sigma-Aldrich
Acetic acid solution, suitable for HPLC
Sigma-Aldrich
Acetic acid, for luminescence, BioUltra, ≥99.5% (GC)
Sigma-Aldrich
Acetic acid, glacial, ACS reagent, ≥99.7%
Sigma-Aldrich
Acetic acid, glacial, puriss., 99-100%
Sigma-Aldrich
Acetic acid, glacial, puriss., meets analytical specification of Ph. Eur., BP, USP, FCC, 99.8-100.5%
Sigma-Aldrich
Acetic acid, glacial, ReagentPlus®, ≥99%
Sigma-Aldrich
Acetic acid, glacial, ≥99.99% trace metals basis
Sigma-Aldrich
Acetic acid, glacial, puriss. p.a., ACS reagent, reag. ISO, reag. Ph. Eur., ≥99.8%
Supelco
5α-Androstan-17β-ol-3-one, VETRANAL®, analytical standard
Millipore
Bifido Selective Supplement B, suitable for microbiology
Sigma-Aldrich
Hydrazine solution, 1 M in acetonitrile
Sigma-Aldrich
Hydrazine solution, 35 wt. % in H2O
Sigma-Aldrich
Hydrazine solution, 1.0 M in THF
Sigma-Aldrich
5α-Androstan-17β-ol-3-one, purum, ≥99.0% (TLC)
Sigma-Aldrich
5α-Androstan-17β-ol-3-one, ≥97.5%
USP
Glacial acetic acid, United States Pharmacopeia (USP) Reference Standard
Sigma-Aldrich
Hydrazine solution, 1.0 M in ethanol