Inter-laboratory study on formaldehyde determination by HPLC

Abstract

The colorimetric determination of formaldehyde in a water extract of a leather sample is a procedure that has been criticized because of possible interferences of other aldehydes and coloured substances that could interfere in the spectrophotometric detection. The measurement by liquid chromatography HPLC is an alternative method that was developed some years ago. This method is more sophisticated but more selective and free of the aforementioned interferences. It is not sensitive to coloured extracts. With the implementation of HPLC equipment in many laboratories, this choice has become feasible in our sector. The process is selective. Formaldehyde is separated and quantified as a derivative from other aldehydes and ketones by liquid chromatography. The free-formaldehyde and formaldehyde which is hydrolysed during extraction to yield free-formaldehyde are detected by this method. The sample is eluted with water at 40ºC. The eluate is mixed with 2,4 dinitrophenylhydrazine, whereby aldehydes and ketones react to yield the respective hydrazones. These are separated by means of a reversed-phase HPLC method, detected at 350 nm and quantified. The aim of this work is to present a collaborative inter-laboratory study coordinated by the Igualada Leather Technology School and carried out with four other laboratories that had previosly implemented the HPLC method or that were planning to do this. Determination of formaldehyde content in leather was carried out in each laboratory in accordance with prEN ISO 17226:2005 - HPLC Standard, developed by the Committee CEN/TC 289. Part 2 of the ISO 5725 Standard (Basic method for the determination of repeatability and reproducibiliry of a standard measurement method) was applied to examine the results. The study proved successful. The HPLC method achieved very reproducible results between laboratories. This work has also demonstrated that other aldehydes, glutaraldehyde included, do not interfere in the chromatographic method. The use of a PDA detector increases the confidence of the detection of formaldehyde in leather samples