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Sensitive determination of organic acid preservatives in juices and soft drinks treated by monolith-based stir cake sorptive extraction and liquid chromatography analysis.

Analytical and bioanalytical chemistry (2013-01-12)
Fuhua Lin, Shuyu Nong, Xiaojia Huang, Dongxing Yuan
ABSTRACT

A simple, efficient, and sensitive method for simultaneous determination of sorbic acid (SA), benzoic acid (BA), and cinnamic acid (CA) in juices and soft drinks was developed by stir cake sorptive extraction (SCSE) coupling to high-performance liquid chromatography with diode array detection. The SCSE based on polymeric ionic liquid-based monolith (PILM) as extractive medium was used to concentrate these three organic acid preservatives. Because hydrophobic and ion-exchange interactions co-contributed to the extraction, the PILM-SCSE exhibited a high extractive capability towards analytes. To obtain optimum extraction performance, several SCSE parameters were investigated and discussed, including desorption solvent, pH value, ionic strength in the sample matrix, and the extraction and desorption time. Under the optimized extraction conditions, limits of detection of 0.16, 1.08, and 0.18 μg/L (S/N=3) and quantification limits of 0.52, 3.42, and 0.61 (S/N=10) were obtained for SA, BA, and CA, respectively. The method also showed good linearity and reproducibility, as well as advantages such as simplicity, low cost, and high feasibility. Finally, the proposed method was successfully applied to the determination of SA, BA, and CA in real juices and soft drinks, and the recoveries ranged from 63.0 to 107 %.

MATERIALS
Product Number
Brand
Product Description

Sigma-Aldrich
Sorbic acid, ≥99.0%
Sigma-Aldrich
Benzoic acid, meets analytical specification of Ph. Eur., BP, USP, FCC, E210, 99.5-100.5% (alkalimetric)
Sigma-Aldrich
Sorbic acid, tested according to Ph. Eur.
Supelco
Benzoic acid, certified reference material for titrimetry, certified by BAM, ≥99.5%
Supelco
trans-Cinnamic acid, analytical standard
Supelco
Benzoic acid, Pharmaceutical Secondary Standard; Certified Reference Material
Sorbic acid, European Pharmacopoeia (EP) Reference Standard
Supelco
Melting point standard 121-123°C, analytical standard
Sigma-Aldrich
Benzoic acid, SAJ first grade, ≥99.5%
Sigma-Aldrich
Sorbic acid, SAJ first grade, ≥98.5%
Sigma-Aldrich
Benzoic acid, SAJ special grade, ≥99.5%
Sigma-Aldrich
trans-Cinnamic acid, 97%
Sigma-Aldrich
Potassium benzoate, ReagentPlus®, 99%
Sigma-Aldrich
Benzoic acid, ReagentPlus®, 99%
Sigma-Aldrich
Benzoic acid, natural, ≥99.5%, FCC, FG
Sigma-Aldrich
Benzoic acid, ≥99.5%, FCC, FG
Sigma-Aldrich
trans-Cinnamic acid, ≥99%
Sigma-Aldrich
Benzoic acid, ACS reagent, ≥99.5%
Sigma-Aldrich
2,4-Hexadienoic acid, ≥99%, FCC
Sigma-Aldrich
Benzoic acid, puriss. p.a., ACS reagent, reag. Ph. Eur., ≥99.9% (alkalimetric)
Sigma-Aldrich
Benzoic acid, purified by sublimation, ≥99%
Sigma-Aldrich
trans-Cinnamic acid, natural, ≥99%, FCC, FG
Sigma-Aldrich
trans-Cinnamic acid, ≥99%, FG
Supelco
SS Benzoic Acid, 2000 μg/mL in dichloromethane, analytical standard
Supelco
Benzoic acid, Standard for quantitative NMR, TraceCERT®
Supelco
Mettler-Toledo Calibration substance ME 18555, Benzoic acid, analytical standard, for the calibration of the thermosystem 900, traceable to primary standards (LGC)