The Determination of Semicarbazide (N-Aminourea) in Commercial Bread Products by Liquid Chromatography−Mass Spectrometry

Abstract

Recently, semicarbazide has been found in food in jars sealed with cap liners that were manufactured using azodicarbonamide as a blowing agent. These reports raised the concern that the use of azodicarbonamide-an approved dough conditioner-may result in semicarbazide residues in bread. To answer this question, a method based upon the previously reported liquid chromatography/tandem mass spectrometry determination of the semicarbazone of o-nitrobenzaldehyde was utilized. The method adopted for this work includes an extensive cleanup and reaction with o-nitrobenzaldehyde at pH 3.5, rather than with the widely used 0.1 M HCl, to form the semicarbazone derivative. A stable isotope dilution assay was used to determine the free semicarbazide present in the bread products. Levels of semicarbazide ranged from 10 to 1200 ppb in commercial bread products with azodicarbonamide listed among their ingredients.

Semicarbazide in Canadian bakery products

“…These values are lower than those reported by Noonan et al (2005) in the USA (260 and 180, respectively), especially while taking into account that method described in this paper analyses both 'free' and 'bound' SC, while the other only the 'free' one. This difference is perhaps due to the large percentage of 'white flour' type bakery products used by Noonan et al, but both studies point to a large variation in SC concentration in baking goods.…”

“…Lastly, results from flour spiking studies with ADA (Becalski et al 2004) and the results from baking bread from flour spiked at maximum allowable amount of ADA (45 mg kg À1 of flour) (Noonan et al 2005) tentatively indicate that that manufacturers might be following Food and Drug Regulations on the use of ADA as a baking additive.…”

“…The procedure of measuring not only free, but also hydrolysable SC was used because the acid hydrolysis condition employed in an analytical method is not dissimilar to human gastric environment. When the experimental work was completed, the paper dealing with concentration of SC in US bakery products (Noonan et al 2005) was published. Noonan et al extracted bread and bun samples with pure water and measured the content of free SC in that extract.…”

A Rapid and Sensitive Method for Semicarbazide Screening in Foodstuffs by HPLC with Fluorescence Detection

“…The SEM extraction was carried out according to previous publications with minor modifications (Becalski et al 2004;Noonan et al 2005;Ye et al 2011). A variety of commercial products were purchased from local food stores.…”

An ultrasensitive competitive immunochromatographic assay (ICA) based on surface-enhanced Raman scattering (SERS) for direct detection of 3-amino-5-methylmorpholino-2-oxazolidinone (AMOZ) in tissue and urine samples

“…Many methods for the detection of FTD and AMOZ have been developed, such as Page 4 of 32 A c c e p t e d M a n u s c r i p t 4 HPLC-UV [13], LC-MS [14] and LC-MS/MS [15,16]. These analytical methods have many advantages of quantitative nature, precision and accuracy; however, they require expensive equipment, skilled analysts and time-consuming sample preparation steps.…”