A derivatization approach using pyrylium salts for the sensitive and simple determination of sulfide in spring water by high performance liquid chromatography.

A derivatization approach using pyrylium salts for the sensitive and simple determination of sulfide in spring water by high performance liquid chromatography.

Journal of chromatography. A (2015-07-15)

Żaneta Rembisz, Dorota Bzdurska, Justyna Obiedzińska, Ramón Martínez-Máńez, Robert Zakrzewski

ABSTRACT

A high-performance liquid chromatography method based on pre-column derivatization with the pyrylium salts (4-[p-(N,N-dimethylamino)phenyl]-2,6-diphenylpyrylium perchlorate (LN1) and 2,4,6-triphenylpyrylium tetrafluoroborate (L1)) has been developed for the determination of sulfide. After the reaction of sulfide ions with LN1 or L1 aiming at the formation of the corresponding thiopyrylium derivatives LN3 or L3, they were separated on a C18 column using phosphate buffer and acetonitrile as eluent, and afterwards detected with a UV/vis detector. By using the described method, sulfide ions can be determined in the range of 5.12-486.4 μg·L(-1) or 1.024-20.48 μg·L(-1) by means of L1 or LN1, respectively. In our experiments, the relative standard deviation was not higher than 2% and the recovery coefficient was in the range of 88-102%. The proposed method was applied to the determination of sulfide in spring water samples from Busko Zdrój and Uniejów health resorts located in Poland.

MATERIALS

Product Number

Brand

Product Description

13-1640

Sigma-Aldrich

Hydrochloric acid, JIS special grade, 35.0-37.0%

13-1760

Sigma-Aldrich

Hydrochloric acid solution, 0.01 M

13-1710

Sigma-Aldrich

Hydrochloric acid solution, 0.5 M

13-1683

Sigma-Aldrich

Hydrochloric acid solution, 12 M

13-1740

Sigma-Aldrich

Hydrochloric acid solution, 0.05 M

13-1686

Sigma-Aldrich

Hydrochloric acid solution, 6 M

13-1790

Sigma-Aldrich

Hydrogen chloride – ethanol solution, 0.1 M in ethanol

13-1690

Sigma-Aldrich

Hydrochloric acid solution, 2 M

13-1700

Sigma-Aldrich

Hydrochloric acid solution, 1 M

609773

Sigma-Aldrich

Sodium phosphate monobasic-¹⁶O₄, 99.9 atom % ¹⁶O

679186

Sigma-Aldrich

Acetonitrile solution, contains 0.05 % (w/v) ammonium formate, 5 % (v/v) water, 0.1 % (v/v) formic acid, suitable for HPLC

705551

Sigma-Aldrich

Hydrogen chloride solution, 3 M in cyclopentyl methyl ether (CPME)

699608

Sigma-Aldrich

Phosphoric acid solution, NMR reference standard, 85% in D₂O (99.9 atom % D), NMR tube size 3 mm × 8 in.

698822

Sigma-Aldrich

Phosphoric acid solution, NMR reference standard, 85% in D₂O (99.9 atom % D), NMR tube size 5 mm × 8 in.

W530574

Sigma-Aldrich

Hydrochloric acid solution, 32 wt. % in H₂O, FCC

13-1720

Sigma-Aldrich

Hydrochloric acid solution, 0.2 M

13-1650

Sigma-Aldrich

Hydrochloric acid, SAJ first grade, 35.0-37.0%

13-1750

Sigma-Aldrich

Hydrochloric acid solution, 0.02 M

272345

Sigma-Aldrich

2,4,6-Triphenylpyrylium tetrafluoroborate, 98%

574732

Sigma-Aldrich

Acetonitrile solution, contains 0.1 % (v/v) trifluoroacetic acid, suitable for HPLC

574724

Sigma-Aldrich

Acetonitrile solution, contains 0.05 % (v/v) trifluoroacetic acid

576956

Sigma-Aldrich

Acetonitrile solution, contains 0.1 % (v/v) formic acid, suitable for HPLC

612162

Sigma-Aldrich

Phosphoric acid solution, NMR reference standard, 85% in D₂O (99.9 atom % D), NMR tube size 4.2 mm × 8 in. , WGS-5BL Coaxial NMR tube

W290017

Sigma-Aldrich

Phosphoric acid solution, 85 wt. % in H₂O, FCC, FG

H1758

Sigma-Aldrich

Hydrochloric acid, 36.5-38.0%, BioReagent, for molecular biology

685461

Sigma-Aldrich

Acetonitrile solution, contains 10.0% acetone, 0.05% formic acid, 40.0% 2-propanol

84429

Sigma-Aldrich

Hydrochloric acid solution, ~6 M in H₂O, for amino acid analysis

H9892

Sigma-Aldrich

Hydrochloric acid solution, 1.0 N, BioReagent, suitable for cell culture

2104

Supelco

Hydrochloric acid solution, volumetric, 0.1 M HCl (0.1N), endotoxin free

675415

Sigma-Aldrich

Acetonitrile, HPLC Plus, ≥99.9%, poly-coated bottles