Skip to Content
Merck
  • Microextraction by packed sorbent (MEPS) to analyze catecholamines in innovative biological samples.

Microextraction by packed sorbent (MEPS) to analyze catecholamines in innovative biological samples.

Journal of pharmaceutical and biomedical analysis (2014-12-17)
Maria Addolorata Saracino, Laura Santarcangelo, Maria Augusta Raggi, Laura Mercolini
ABSTRACT

A new microextraction by packed sorbent (MEPS) procedure coupled to a high-performance liquid chromatographic method has been developed for quantitation of catecholamines (i.e. norepinephrine, epinephrine and dopamine) in innovative biological samples, namely dried plasma and urine spots. Analyses were carried out on a C18 reversed-phase column using a mobile phase composed of 2.5% methanol and 97.5% aqueous citrate buffer, containing octanesulfonic acid. Coulometric detection was used, setting the first analytical cell at -0.350 V and the second analytical cell at +0.400 V. Dried matrices were purified by means of a fast and feasible MEPS procedure, optimized on C18 sorbent and requiring only a small amount of biological sample. The availability of miniaturized procedures allowed satisfying specific requirements that ought to be considered during pre-treatment intended for catecholamine analysis. The extraction yield values were always higher than 85% and sensitivity was good, with a limit of quantitation of 100 pg mL(-1) for all the analytes. Satisfactory results were also obtained in terms of linearity, precision and accuracy. The method was successfully applied to dried plasma and urine spots derived from two socially diversified groups, namely psychiatric patients and poly-drug abusers, in comparison to healthy volunteers.

MATERIALS
Product Number
Brand
Product Description

Sigma-Aldrich
Sodium hydroxide, BioXtra, ≥98% (acidimetric), pellets (anhydrous)
Sigma-Aldrich
Potassium chloride, anhydrous, free-flowing, Redi-Dri, ReagentPlus®, ≥99%
Sigma-Aldrich
Sodium hydroxide, puriss., meets analytical specification of Ph. Eur., BP, NF, E524, 98-100.5%, pellets
Sigma-Aldrich
Potassium chloride, puriss. p.a., ≥99.5% (AT)
Sigma-Aldrich
Ammonium chloride, puriss., meets analytical specification of Ph. Eur., BP, USP, FCC, 99.5-100.5% (calc. to the dried substance)
Sigma-Aldrich
Sodium metabisulfite, puriss., meets analytical specification of Ph. Eur., BP, NF, FCC, E223, dry, 97-100.5%
Sigma-Aldrich
Methanol, ACS reagent, ≥99.8%
Sigma-Aldrich
Methanol, Absolute - Acetone free
Sigma-Aldrich
Sodium hydroxide solution, 5.0 M
Sigma-Aldrich
Sodium hydroxide, puriss. p.a., ACS reagent, K ≤0.02%, ≥98.0% (T), pellets
Sigma-Aldrich
Potassium chloride, ReagentPlus®, ≥99.0%
Sigma-Aldrich
Potassium chloride, ACS reagent, 99.0-100.5%
Sigma-Aldrich
Methanol, suitable for HPLC, ≥99.9%
Sigma-Aldrich
Hydrogen chloride solution, 3 M in cyclopentyl methyl ether (CPME)
Sigma-Aldrich
Methanol, NMR reference standard
Supelco
Sodium hydroxide concentrate, 0.1 M NaOH in water (0.1N), Eluent concentrate for IC
Sigma-Aldrich
Sodium phosphate dibasic solution, BioUltra, 0.5 M in H2O
Sigma-Aldrich
Sodium chloride solution, 0.85%
Sigma-Aldrich
Phosphoric acid solution, NMR reference standard, 85% in D2O (99.9 atom % D), NMR tube size 3 mm × 8 in.
Sigma-Aldrich
Hydrochloric acid solution, 32 wt. % in H2O, FCC
Sigma-Aldrich
Phosphoric acid solution, NMR reference standard, 85% in D2O (99.9 atom % D), NMR tube size 5 mm × 8 in.
Sigma-Aldrich
Hydrochloric acid solution, ~6 M in H2O, for amino acid analysis
Sigma-Aldrich
Ammonia, puriss., anhydrous, ≥99.95%
Sigma-Aldrich
Pyrocatechol, purified by sublimation, ≥99.5%
Sigma-Aldrich
Potassium chloride, 99.999% trace metals basis
Sigma-Aldrich
Methanol, anhydrous, 99.8%
Sigma-Aldrich
3-Ethyl-2,4-pentanedione, mixture of tautomers, 98%
Sigma-Aldrich
Sodium chloride, BioUltra, for molecular biology, ≥99.5% (AT)
Supelco
Hydrogen chloride – ethanol solution, ~1.25 M HCl, for GC derivatization, LiChropur
Supelco
Hydrogen chloride – 2-propanol solution, ~1.25 M HCl (T), for GC derivatization, LiChropur