Simultaneous Extraction and Determination of Preservatives and Antioxidants in Juice Samples by an Optimized Microextraction Method Using Central Composite Design and Validated with Accuracy Profile.

>

Background

Food additives are widely used in industries. Overall, these additives have a beneficial role, but if their concentration exceeds certain limits, they may have an adverse effect on human health.

Objective

This study outlines the determination of benzoic acid (BA), sorbic acid (SA), butylated hydroxyanisole (BHA), and butylated hydroxytoluene (BHT) in juices using dispersive liquid-liquid microextraction and HPLC-diode-array detection.

Methods

Different parameters that significantly affect the extraction efficiency were optimized. The disperser and extraction solvents were acetone and chloroform, respectively. The other parameters were selected and optimized using two-level (2k) factorial and central composite designs, respectively. A full method validation using an accuracy profile for the total measurement error was carried out.

Results

The optimized conditions were 625 μL acetone, 350 μL chloroform, 0.85 g NaCl, and pH 2. The validated method demonstrated good linearity with R² ≥ 0.99 and good precision with the RSD of repeatability and intermediate precision at 1.97-10.7% and 2.31-11.9%, respectively. The relative recoveries were 96.2-105.4%, and the LODs were around 0.03 μg/mL for all compounds. The analysis of 41 samples revealed that BA and SA were quantified in 25 and 20 samples, respectively. BHA and BHT were not detected.

Conclusions

The proposed methodology is an appropriate tool to determine important food additives in juices to ensure their compliance with the food additives legislation. Highlights: The work has demonstrated that the method can be successfully used in the simultaneous determination of four food additives in fruit juices.