Abstract

A simple and rapid method for the quantitation of total fat in olive samples is designed, evaluated, and presented. This method is based on an innovative closed-vessel microwave-assisted extraction (MAE) technique. A method was designed for olives, and some figures of merits were evaluated: limit of detection (LOD), limit of quantification (LOQ) and expanded uncertainty (U). The data obtained in these experiences show that the workflow of the MAE method in a closed container is statistically equivalent to the other two methods, showing in this case better performance indicators (LOD = 0.02%, LOQ = 0.06%, and U = 15%). In addition, it is also demonstrated that the complete MAE method workflow allows the determination of total fat in a maximum of 12 analyses simultaneously for about 100 min in each run, which is the capacity of the rotor. This is a much better productivity when compared to the traditional Soxhlet-based method. Considering the sample workflow, the closed-vessel MAE method greatly simplifies sample handling, therefore minimizing sample loss during sample preparation and reducing analysis time. When MAE is compared to NIR-based methods, the advantage comes from there being no need for any type of calibration in the sample matrix. The MAE method itself can be used to determine the reference value for NIR calibration purposes. The results obtained for CRM using MAE were equivalent to the ones shown on the certificate.

Highlights

  • The objective of this study is to evaluate and compare the capabilities of a new workflow with a microwave-assisted extraction method for olive samples to determine their total fat content

  • It has already been verified that the microwave-assisted extraction (MAE) workflow had statistical equivalence with a validated or referential method

  • MAE results were compared against Soxhlet results

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Summary

Introduction

Consumers are concerned about fat ingestion. As fat affects the texture and taste of food, and considering the change of food habits, the potential risk of consuming excess calories from fat is considerable. On the other hand, include all the “fatty” materials in a food (i.e., generally those materials dissolved in a fat-solubilizing solvent) This includes sterols, mono, di, and triglycerides, phospholipids, glycolipids, free fatty acids, fat soluble vitamins, etc. To clarify some of the terminologies, the Food and Drug Administration, in Chapter 21 of CFR 101.9NUTRITION LABELING OF FOOD, defines fat as the sum of the fatty acids in the food, regardless of source, that are expressed as triglyceride equivalents. These fatty acids may be present as free fatty acids, mono, di, and triglycerides, phospholipids, glycolipids, or sterol lipids. These classifications include saturated, monounsaturated, polyunsaturated, and trans fatty acids [1]

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