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FORMALDEHYDE - ARC Sciences

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APPLICATION NOTE<br />

As of: April, 2010<br />

<strong>FORMALDEHYDE</strong><br />

Formaldehyde is used for the disinfection of<br />

industrially manufactured products. However, it is detrimental<br />

to health and its potential carcinogenicity led<br />

to the current utilization of formaldehyde donors for<br />

microbiological long-term stabilization, which are in<br />

hydrolytic equilibrium with formaldehyde. Thereby, the<br />

concentration of free formaldehyde is kept as low as<br />

possible.<br />

The quantitative determination of free formaldehyde<br />

seems quite problematic. Firstly, the detection characteristics<br />

of formaldehyde are very unfavorable. Consequently,<br />

derivatization is necessary in order to<br />

achieve the required sensitivity. Secondly, the hydrolytic<br />

equilibrium between donor and free formaldehyde<br />

can change quite quickly, which makes the preparation<br />

of samples more difficult and/or influences the<br />

correctness of analytical results.<br />

An elegant solution for this problem is, therefore, to<br />

perform the derivatization step after separation on an<br />

HPLC column, because the equilibrium cannot be influenced<br />

when donor and free formaldehyde are<br />

chromatographically separated before derivatization. PICKERING offers the complete post-column<br />

derivatization system PINNACLE PCX for the detection of traces of formaldehyde. The user, however,<br />

has to supply columns, eluents, reagents, etc..<br />

Description of the Method<br />

The derivatization of formaldehyde is performed in a one-step reaction using acetyl acetone<br />

(2,4-pentanedione). In the presence of an ammonium salt, it reacts to a yellow, strongly fluorescing<br />

3,5-diacetyl-1,4-dihydrolutidine derivative. The detection is performed with either a UV/VIS or fluorescence<br />

detector.<br />

LCTech GmbH I P.O. Box 1360 I 84403 Dorfen, Germany Seite 1 von 3<br />

Tel: +49-(0)8081-9368-0 I Fax: +49-(0)8081-9368-10 I www.Lctech.de I info@Lctech.de


APPLICATION NOTE<br />

HPLC Conditions and Derivatization Parameters<br />

HPLC<br />

Operating Mode<br />

Isocratic<br />

Eluent Acetonitrile:water (85:15)<br />

Degassing<br />

HPLC Column<br />

Helium- or vacuum degassed<br />

RP C18<br />

Column Oven 40 °C<br />

Flow Rate<br />

0.5 mL/min<br />

Post-column Derivatization<br />

Pinnacle PCX<br />

Single-pump<br />

Reactor volume 500 µL<br />

Reactor temperature 100 °C<br />

Reagents 0.81 M Ammonium acetate /<br />

0.12 M Glacial acetic acid (pH=5)/<br />

0.05 M 2,4-Pentanedione with water<br />

Reagent Flow<br />

0,4 mL/min<br />

Detection<br />

Detection Mode<br />

Excitation Wavelength<br />

Emission Wavelength<br />

Flow cell<br />

Fluorescence detection<br />

412 nm<br />

510 nm<br />

Analytic; pressure stable up to 7 bar<br />

LCTech GmbH I P.O. Box 1360 I 84403 Dorfen, Germany Seite 2 von 3<br />

Tel: +49-(0)8081-9368-0 I Fax: +49-(0)8081-9368-10 I www.Lctech.de I info@Lctech.de


APPLICATION NOTE<br />

Chromatogram<br />

Chromatogram of a shampoo sample<br />

Sample spiked with 0,05% formaldehyde. Determination according to K 84.00-7(EG)<br />

Literature<br />

1) J. Meister, H. Engelhardt, LaborPraxis 1995, 7, 28 – 31.<br />

2) Amtliche Sammlung §64 LFGB, K 84.00-7(EG), September 1991.<br />

3) EU method for analysis of formaldehyde in cosmetics (Second Commission Directive<br />

82/434/EEC, Annex IV, Identification and Determination of free formaldehyde)<br />

Order Information<br />

Order Number<br />

Description<br />

1153-1022 PINNACLE PCX – single-pump; 500 µL reactor<br />

LCTech GmbH I P.O. Box 1360 I 84403 Dorfen, Germany Seite 3 von 3<br />

Tel: +49-(0)8081-9368-0 I Fax: +49-(0)8081-9368-10 I www.Lctech.de I info@Lctech.de

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