Method development and validation studies for simultaneous GC-MS / FID determination of erucic acid in foods

It is thought that the high percentage of Erucic Acid, also known as omega-9 fats, in foods poses certain health risks. It has been reported in the literature that people exposed to erucic acid levels experience cardiovascular disorders, susceptibility to myocardial fat, increased rates of diabetes, and minimal renal excretion. For this reason, the American Food and Drug Administration (FDA) has some regulations regarding the amount of Erucic Acid in Foods and in our country, the Turkish Food Codex C ommuniqué on Erucic Acid is restricted to 5% in foods and 1% of total fat content in baby formula foods. Turkish Food Codex Communiqué on Sampling and Analysis Method Criteria for Official Control of Erucic Acid Level in Certain Foods (Communiqué NO: 2016/4) has been published. In this study conducted within the framework of Communiqué No 2016/4, GCMS FID analysis method, which will work simultaneously, was developed. There is matrix effect in food analysis. Therefore, there is a possibility of peaks of other analytes at the time of arrival of erucic acid. Although Erucic acid is given as a standard; Since the GCoperating conditions remain unchanged, the time of arrival of the analyte is determined. Here it needs to be verified with the MS detector. The oils of the foods with Erucic Acid were extracted by soxelet method and the Fatty Acid composition and the amount of Erucic Acid of the extracted oils were examined. The products are supplied to the GC device with MS and FID detector. Simultaneous verification of erucic acid detected in MS and FID detector in MS detector and calculation in FID detector was performed. In this method, LOD, LOQ, reproducibility, reproducibility, retrieval and accuracy studies were performed. In the study, LOD was found to be 0.11%, LOQ was 0.38% and MDL was 0.11%. The suitability of these values was checked at 5 different points. According to the Turkish Commercial Code 2016/4 Communiqué on Sampling and Analysis Method Criteria for Official Control of Erucic Acid Level in Certain Foods LOD OD1 g / kg (≤0.1%); The LOQ is ≤5 g / kg (≤0.5%). In the recovery studies, the recovery rates ranged from 98.84% to 100.30%. In the study, recovery showed good analytical performance and results obtained at three different concentrations. In the repeatability study, the combined% RSDr (pool) for fat and oil studies at different concentrations was calculated as 1.66% and 1.40%, respectively. Since these results were smaller than 1.91% HRSDr%, the combined relative standard deviation was considered appropriate. In the reproducibility study, the combined% RSDR (pool) for fat and oil studies at different concentrations was calculated as 2.13% and 2.51%, respectively. Since these results were smaller than the 2.88% HRSDR, the combined relative standard deviation was evaluated. It is important when comparing measurement results and deciding on compliance with limits. In the validation study for erucic acid analysis, the uncertainty of measurement was found to be extended uncertainty ± 0.60% in the 95% confidence interval of k = 2. All the results found meet the limits given in the Turkish Food Codex Communiqué on the Sampling and Analysis Methods Criteria for Official Control of Erucic Acid Level in Certain Foods (Communiqué No: 2016/4). As a result; In this study, the accuracy rate in detecting the analysis of products with erucic acid was increased and an analysis method related to both analysis and verification of erucic acid was put forward simultaneously. This analysis method has been developed in GC-MS / FID which will work concurrently within the framework of the Turkish Food Codex Communiqué on the Sampling and Analysis Method Criteria for Official Control of Erucic Acid Level in Certain Foods (Communiqué No: 2016/4). Validation studies of this method has been made to be used by laboratories performing erucic acid analysis.