کد مقاله | کد نشریه | سال انتشار | مقاله انگلیسی | نسخه تمام متن |
---|---|---|---|---|
1198739 | 1493470 | 2016 | 7 صفحه PDF | دانلود رایگان |
• Small amounts of sample and reagents for derivatization of fatty acids.
• Fast sample preparation procedure for GC analysis.
• Minor errors due to the shortening of procedure steps.
• Procedure validated for bovine, chicken, pork, fish, and shrimp samples.
• Viability to collect samples without slaughtering of animals.
In order to analyze the composition of fatty acids employing gas chromatography as the separation method, a derivatization of lipids using esterification and transesterification reactions is needed. The methodologies currently available are time consuming and use large amounts of sample and reagents. Thus, this work proposes a new procedure to carry out the derivatization of fatty acids without the need for prior extraction of lipids. The use of small amounts of sample (100 mg) allows the analysis to be performed in specific parts of animals, in most cases without having them slaughtered. Another benefit is the use of small amounts of reagents (only 2 mL of NaOH/Methanol and H2SO4/Methanol). The use of an experimental design procedure (Design Expert software) allows the optimization of the alkaline and acid reaction times. The procedure was validated for five minutes in both steps. The method was validated for bovine fat, beef, chicken, pork, fish and shrimp meats. The results for the merit figures of accuracy (from 101.07% to 109.18%), precision (RSDintra-day (from 0.65 to 3.93%), RSDinter-day (from 1.57 to 5.22%)), linearity (R2 = 0.9864) and robustness confirmed that the new method is satisfactory within the linear range of 2–30% of lipids in the sample. Besides the benefits of minimizing the amount of samples and reagents, the procedure enables gas chromatography sample preparation in a very short time compared with traditional procedures.
Journal: Journal of Chromatography A - Volume 1456, 22 July 2016, Pages 235–241