The proposed extractions were tested to extract the dinitrophenylhydrazone derivatives of the eight aldehydes of interest and five internal standards and four times 1 mL hexane showed the best results. Each aldehyde was considered as positively identified in samples if the ratio between the chromatographic retention time of the analyte and that of the internal standard, i.e., the relative retention time (RRT) of the analyte, corresponded to that of the average retention time of the calibration solutions within a ±2.5% tolerance interval and the peak area ratio of the two transitions of the native analyte corresponded to that of the averaged transition ratio of the calibration solutions within the tolerances set by the Commission Decision 2002/657/EC.21. Six samples of ground Kellogg's® Corn Flakes® cereals were spiked with the internal standards solution and five of them with concentrations ranging from 0.16 to 4.0 mg/kg for 4‐HHE and 4‐HNE, 0.15 to 7.5 mg/kg for MDA, crotonaldehyde, benzaldehyde, 2,4‐decadienal and 2,4‐nonadienal and 0.5 to 12.5 mg/kg for hexanal.

The solvent was then evaporated to dryness in a SpeedVac concentrator (SVC100, Savant Instruments Inc., Farmingdale, NY, USA) and 100 μL of 0.03% acetic acid solution/acetonitrile 60/40 (v/v) was added to the tube. These observations can be explained by the fact that 4‐HHE, 2,4‐decadienal and 2,4‐nonadienal are the three aldehydes quantified by using an internal standard which is not their isotopic analogue or the same molecule with an added methyl group and which has a behaviour different from the one of the analyzed aldehydes. Methylcrotonaldehyde (MeCRT), benzaldehyde‐13C, hexanal‐D12, 4‐HNE‐D3 and methylmalondialdehyde (MeMDA) were used as internal standards in the quantitative analysis. Target spiking levels, mean introduced concentrations (average of the real concentrations for all experiments), LOD, LOQ, repeatability, intermediate precision, recovery, linearity (R2), calibration curve equations, and uncertainty are summarized in Table 2.

Formaldehyde-2,4-DNPH may be used as an analytical standard for the determination of the analyte in air samples, food and feed products, and aquatic products by various chromatography techniques. The best compromise between solubility and chromatographic peak areas was obtained for the 8 aldehydes with a DNPH concentration of 0.05 M in acetonitrile/acetic acid (9/1, v/v).

h�bbd```b``~"W�H�}`70����s@$�3��&�����֫"y>�U� I��{@��� ��D2X�U��d�������`�L� R��� ��Q`���f�����U ���i/���a�����l�����?��� ��� Safety & Documentation. Kellogg's® Corn Flakes® cereals were bought in a local supermarket. 2). The best compromise between solubility and chromatographic peak areas was obtained for the 8 aldehydes with a DNPH concentration of 0.05 M in acetonitrile/acetic acid (9/1, v/v).

Create . Recoveries met the criteria of the European decision 2002/657/EC,18 which is set between 80 and 110% for MDA, 4‐HHE, 4‐HNE, crotonaldehyde, benzaldehyde and hexanal.
Stock solutions of the other aldehydes were prepared by dissolving the compound in water/ethanol 50/50 (v/v). It is a member of phenylhydrazines and a C-nitro compound.

Log in or register to post comments; Tue, 04/07/2009 - 15:50 #2. Profiling of Omega-Polyunsaturated Fatty Acids and Their Oxidized Products in Salmon after Different Cooking Methods. The response (ratio between each aldehyde and the internal standard peak areas) was plotted versus standard concentrations. 2,4-Dnph. The full text of this article hosted at iucr.org is unavailable due to technical difficulties. I know this method well.

The DNPH reagent is highly reactive toward formaldehyde. The measurement uncertainty (MU) (a parameter that characterizes the dispersion of the values that could reasonably be attributed to the measurand) is expressed here as a relative expanded uncertainty (a percentage of the result) and is calculated from the total variance of the β‐expectation tolerance interval, using a coverage factor of 2. At a formaldehyde concentration of 1.2 mg/m. These parameters were determined during experiments conducted over three different days with ground Kellogg's® Corn Flakes® cereals as model matrix for animal feed and spiked at different levels of concentration.
The information in this document is based on the present state of our knowledge and is applicable to the product with regard to appropriate safety precautions. The intra- and intermolecular hydrogen bonds in DNPH have been investigated by vibrational spectroscopic analysis.

Water was of Chromanorm quality, while acetic acid 100% was of Normapur Quality and were both provided by VWR International (West Chester, PA, USA). The reaction can proceed completely with the reaction time in-crease. Knowing that polyunsaturated fatty acids can lead to the formation of potentially toxic aldehydes as secondary oxidation products, an analytical method using liquid chromatography coupled to tandem mass spectrometry (LC‐MS/MS) detection was developed to measure the concentration of eight aldehydes in animal feed: malondialdehyde (MDA), 4‐hydroxy‐2‐nonenal (4‐HNE), 4‐hydroxy‐2‐hexenal (4‐HHE), crotonaldehyde (CRT), benzaldehyde (BNZ), hexanal (HXL), 2,4‐nonadienal, and 2,4‐decadienal. The mobile phase was acetonitrile (solvent A) and 0.03% acetic acid solution (solvent B).

Malondialdehyde, 4‐HHE, 4‐HNE, crotonaldehyde, benzaldehyde, and hexanal can be analyzed in the same run in animal feed with a very good accuracy, with recovery rates ranging from 86 to 109% for a working range going from 0.16 to 12.50 mg/kg.


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