A novel mass spectrometric method for formaldehyde in children's personal‐care products and water via derivatization with acetylacetone

Abstract

The developed method allows for the accurate quantification of formaldehyde in PCPs at levels below those required by a new regulation on children's products in Minnesota. The method includes a derivatization procedure that is newly adapted to HPLC/MS/MS; therefore, structures were proposed for the product ions of the derivative (DDL). Copyright © 2017 John Wiley & Sons, Ltd.

TEMPO‐Mediated Electrochemical N‐demethylation of Opiate Alkaloids

“…LC-MS analysis of the electrochemical oxidation of 1 a in the divided electrochemical cell clearly showed the presence of 1 b and TEMPOH in the anode compartment, supporting the proposed mechanism (see supporting information, Figure SI 9). Moreover, the formaldehyde produced at the anode upon hydrolysis of the hypothesized iminium intermediate was detected using a derivatization with acetylacetone and ammonia forming 3,5diacetyl-1,4-dihydrolutidine (m/z of 194.1), which was detected by LC-MS. [35,46,47] As expected, there was no formaldehyde detected in the cathode compartment (see supporting information, Figure SI 10).…”

ElectrochemicalN-demethylation of tropane alkaloids

“…2) which undergoes a two electron electrochemical oxidation reaction to form an amidinium structure. The produced formaldehyde from the removed methyl group was detected by LC-MS using a simple derivatization method, where acetylacetone reacts with formaldehyde in the presence of ammonium acetate to form the cyclized 3,5-diacetyl-1,4-dihydrolutidine product (m/z of 194.1), 62,63 which can be easily detected by LC-MS analysis (Fig. S12 †).…”

Simple click chemistry‐based derivatization to quantify endogenous formaldehyde in milk using ultra‐high‐performance liquid chromatography/tandem mass spectrometry in selected reaction monitoring mode

“…We have developed a simple click chemistry‐based derivatization reaction using GP for the quantification of endogenous FA in milk samples. Compared with alternative reagents such as DNPH and acetyl acetone, 11,19–21 GP derivatization showed features such as the presence of a pre‐charged moiety that enhances the mass spectrometry signal, use of smaller sample volume, and simpler sample preparation steps suitable for routine analysis. The reaction with GP is rapid, it needs ~60 min for completion.…”

“…Spectroscopic methods using HPLC with UV or fluorescence detection after derivatization have been used for FA quantification in foods, [11][12][13]19 with derivatization with acetyl acetone and 2,4-dinitrophenylhydrazine (DNPH) being widely applied for the estimation of FA using HPLC. 11,[19][20][21] However, these methods lack the required sensitivity and specificity and often a high sample volume is needed. Although the best way to analyze compounds at ng to pg levels in foods is mass spectrometry (MS)-based quantification using stable isotope dilution, a few methods have been developed that use labelled FA as an internal standard for quantification of FA.…”

“…Direct detection of FA is cumbersome, as it has to be derivatized with specific reagents prior to analysis. Spectroscopic methods using HPLC with UV or fluorescence detection after derivatization have been used for FA quantification in foods, 11–13,19 with derivatization with acetyl acetone and 2,4‐dinitrophenylhydrazine (DNPH) being widely applied for the estimation of FA using HPLC 11,19–21 . However, these methods lack the required sensitivity and specificity and often a high sample volume is needed.…”