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Optimized Dispersive Liquid–Liquid Microextraction and Determination of Sorbic Acid and Benzoic Acid in Beverage Samples by Gas Chromatography

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Abstract

A new rapid method for direct determination of trace levels of sorbic and benzoic acids was developed by dispersive liquid–liquid microextraction and gas chromatography with flame ionization detection. In the proposed approach, the separation procedure of sorbic and benzoic acids was performed on a general chromatographic column without any prior derivatization processes. Some effective parameters on the microextraction recovery were studied and optimized utilizing multilevel factorial and central composite experimental designs. The best concurrent extraction efficiency acquired using ethanol and chloroform as dispersive and extraction solvents. Central composite design (CCD) resulted in the optimized values of microextraction parameters as follows: 1.0 mL of dispersive and 0.1 mL of extraction solvents, ionic salt concentration of 50 g L−1 at pH 4. Under optimum conditions, the calibration curve was linear over the range 0.5–20 mg L−1. Relative standard deviation was 11% and 13% for five repeated determinations for sorbic and benzoic acids, respectively. Limits of detection were acquired as 0.2 mg L−1 for sorbic acid and 0.5 mg L−1 for benzoic acid. The average recoveries were 31% and 39% for sorbic and benzoic acids, respectively. The method was successfully applied to the determination of sorbic and benzoic acids as preservatives in beverage samples.

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References

  • Ahmadi F, Assadi Y, Milani Hosseini SMR, Rezaee M (2006) Determination of organophosphorus pesticides in water samples by single drop microextraction and gas chromatography-flame photometric detector. J Chromatogr A 1101:307–312

    Article  CAS  Google Scholar 

  • Ahmadzadeh Kokya T, Ahmadzadeh Kokya B, Farhadi K (2008) Chemometrics: A complicated necessity for today’s chemical education. 20th ICCE, Mauritius

  • Anderson JA (1996) Allergic reactions to food. Crit Rev Food Sci Nutr 36:S19–S38

    Article  CAS  Google Scholar 

  • Bindslev-Jensen C (1998) ABC of allergies, food allergy. Br Med J 316:1299–1302

    Article  CAS  Google Scholar 

  • Bindslev-Jensen J, Peters L, Whittle E, Basketter DA (1998) Susceptibility to skin stinging, non-immunologic contact urticaria and acute skin irritation; is there a relationship. Contact Dermat 38(2):90–95

    Article  Google Scholar 

  • Brown SD, Sum ST, Despagne F (1996) Chemometrics. Anal Chem 68:21–61

    Article  CAS  Google Scholar 

  • Cautreels W, van Cauwenberghe K (1978) Experiments on the distribution of organic pollutants between airborne particulate matter and the corresponding gas phase. Atmos Environ 12:1133–1141

    Article  CAS  Google Scholar 

  • CFCC (2004) Food chemicals codex, 5th edn. Committee on food chemicals codex, The National Academies Press, Washington D.C

  • Chen QC, Wang J (2001) Simultaneous determination of artificial sweeteners, preservatives, caffeine, theobromine and theophylline in food and pharmaceutical preparations by ion chromatography. J Chromatogr A 937:57–64

    Article  CAS  Google Scholar 

  • Cordt T, Kußmaul H (1990) Niedermolekulare carbonsäuren imboden, in der ungesättigten zone und im grundwasser. Vom wasser 74:287–298, in German

    CAS  Google Scholar 

  • Dharmadhikari M (1992) Sorbic acid. Vineyard Vintage View Newsletter 7(6):1–5

    Google Scholar 

  • Dobiásová Z, Pazourek J, Havel J (2002) Simultaneous determination of trans-resveratrol and sorbic acid in wine by capillary zone electrophoresis. Electrophoresis 23:263–267

    Article  Google Scholar 

  • Dong C, Wang W (2006) Headspace solid-phase microextraction applied to the simultaneous determination of sorbic and benzoic acids in beverages. Anal Chim Acta 562:23–29

    Article  CAS  Google Scholar 

  • Down S (2006) Ternary extraction system achieves results in seconds. John Wiley & Sons available at: <http://www.separationsnow.com> Last accessed on 8 February 2009

  • EPCD (1995) European parliament and council directive on food additives other than colours and sweeteners. No. 2001/5/EC

  • Gemperline P (2006) Practical guide to chemometrics 2nd edn. CRC, Boca Raton

    Book  Google Scholar 

  • González M, Gallego M, Valcárcel M (1999) Gas chromatographic flow method for the preconcentration and simultaneous determination of antioxidant and preservative additives in fatty foods. J Chromatogr A 848:529–536

    Article  Google Scholar 

  • Guarino G, Fuselli F, Mantia AL, Longo L (2011) Development of an RP-HPLC method for the simultaneous determination of benzoic acid, sorbic acid, natamycin and lysozyme in hard and pasta filata cheeses. Food Chem. doi:10.1016/j.foodchem.2011.01.086

    Google Scholar 

  • Han F, He YZ, Li L, Fu GN, Xie HY, Gan WE (2008) Determination of benzoic acid and sorbic acid in food products using electrokinetic flow analysis-ion pair solid phase extraction-capillary zone electrophoresis. Anal Chim Acta 618:79–85

    Article  CAS  Google Scholar 

  • Helmig D, Müller J, Klein W (1989) Volatile organic substances in a forest atmosphere. Chemosphere 19:1399–1412

    Article  CAS  Google Scholar 

  • Horwitz W (2002) Official methods of analysis of AOAC international 17th edn. AOAC International, Gaithersburg

    Google Scholar 

  • Jalal MAF, Read DJ (1983) The organic acid composition of Calluna heathland soil with special reference to phyto-and fungitoxicity. Plant Soil 70:257–272

    Article  CAS  Google Scholar 

  • Jeannot MA, Cantwell FF (1996) Solvent microextraction into a single drop. Anal Chem 68:2236–2240

    Article  CAS  Google Scholar 

  • Jeannot MA, Cantwell FF (1997) Mass transfer characteristics of solvent extraction into a single drop at the tip of a syringe needle. Anal Chem 69:235–239

    Article  CAS  Google Scholar 

  • Jiang X, Oh SY, Lee HK (2005) Dynamic liquid–liquid–liquid microextraction with automated movement of the acceptor phase. Anal Chem 77:1689–1695

    Article  CAS  Google Scholar 

  • Kawamura K, Ng LL, Kaplan IR (1985) Determination of organic acids in the atmosphere, motor exhausts, and engine oils, IPCS guidelines for the monitoring of genotoxic effects of carcinogens in humans. Environ Sci Technol 19:1082–1086

    Article  CAS  Google Scholar 

  • Kozani RR, Assadi Y, Shemirani F, Milani Hosseini MR, Jamali MR (2007) Part-per-trillion determination of chlorobenzenes in water using dispersive liquid-liquid microextraction combined gas chromatography-electron capture detection. Talanta 72:387–393

    Article  CAS  Google Scholar 

  • Lahti A, Pylvanen V, Hannuksela M (1995) Immediate irritant reactions of benzoic acid are enhanced in washed skin areas. Contact Dermat 33:177–182

    Article  CAS  Google Scholar 

  • Luca C, Passi S, Quattrucci E (1995) Simultaneous determination of sorbic acid, benzoic acid and parabens in foods: a new gas chromatography-mass spectrometry technique adopted in a survey on Italian foods and beverages. Food Addit Contam 12:1–7

    Article  Google Scholar 

  • Lunde G, Gehter J, Gjos N, Lande MBS (1977) Organic micropollutants in precipitation in Norway. Atmos Environ 11:1007–1014

    Article  CAS  Google Scholar 

  • Mandrou B, Nolleau V, Gastaldi E, Fabre H (1998) Solid-phase extraction as a clean-up procedure for the liquid chromatographic determination of benzoic and sorbic acids in fruit-derived products. J Liq Chromatogr Relat Technol 21:829–842

    Article  CAS  Google Scholar 

  • Merck Co (2001) The Merck index 13th edn. [on CD-ROM]

  • Meyers RA (2008) Encyclopedia of analytical chemistry: applications, theory and instrumentation. Wiley, New York

    Google Scholar 

  • Ötles S (2005) Methods of analysis of food components and additives. CRC, Boca Raton

    Book  Google Scholar 

  • Pan Z, Wang L, Mo W, Wang C, Hu W, Zhang J (2005) Determination of benzoic acid in soft drinks by gas chromatography with on-line pyrolytic methylation technique. Anal Chim Acta 545:218–223

    Article  CAS  Google Scholar 

  • Parke DV, Lewis DVF (1992) Safety aspects of food preservatives. Food Addit Contam 9:561–577

    Article  CAS  Google Scholar 

  • Pylypiw HM, Grether MT (2000) Rapid high-performance liquid chromatography method for the analysis of sodium benzoate and potassium sorbate in foods. J Chromatogr A 883:299–304

    Article  CAS  Google Scholar 

  • Rezaee M, Assadi Y, Milani Hosseini MR, Aghaee E, Ahmadi F, Berijani S (2006) Determination of organic compounds in water using dispersive liquid-liquid microextraction. J Chromatogr A 1116:1–9

    Article  CAS  Google Scholar 

  • Rezaei F, Bidari A, Birjandi AP, Milani Hosseini MR, Assadi Y (2008) Development of a dispersive liquid–liquid microextraction method for the determination of polychlorinated biphenyls in water. J Hazard Mater 158:621–627

    Article  CAS  Google Scholar 

  • Saad B, Bari MF, Saleh MI (2005) Simultaneous determination of preservatives (benzoic acid, sorbic acid, methylparaben and propylparaben) in foodstuffs using high-performance liquid chromatography. J Chromatogr A 1073:393–397

    Article  CAS  Google Scholar 

  • Scholz W, Kortmann W (1991) In: Elvers B, Hawkins S, Schulz G (eds) Ullmann’s encyclopedia of industrial chemistry. Wiley, Weinheim

    Google Scholar 

  • Schou L, Krane JE (1981) Organic micropollutants in a Norwegian water-course. Sci Total Environ 20:277–286

    Article  CAS  Google Scholar 

  • Stephan DD, Werner J, Yeater RP (2001) Essential regression and experimental design for chemists and engineers, MS Excel Add-in Software Package

  • Techakriengkrai I, Surakarnkul R (2007) Analysis of benzoic acid and sorbic acid in Thai rice wines and distillates by solid-phase sorbent extraction and high-performance liquid chromatography. J Food Compos Anal 20:220–225

    Article  CAS  Google Scholar 

  • UNEP (2001) Benzoates, SIDS initial assessment report for 13th SIAM, Netherlands, available online at: <http://www.inchem.org/documents/sids/sids/BENZOATES.pdf>, last accessed on 14-11-2010

  • USDA (2004) Determination of benzoic acid, sorbic acid, and methyl, ethyl, Propyl, and Butyl Parabens by HPLC. Food Safety and Inspection Service, Office of Public Health Science, SOP No: CLG-BSP.01

  • USFR (2002) United States Federal Regulations. 21st Code, Part 172

  • Vogt T, Landthaler M, Stolz W (1999) Sodium benzoate induced acute leukocytoclastic vasculitis with unusual clinical appearance. Arch Dermatol 135:726–727

    Article  CAS  Google Scholar 

  • WHO (1999) Safety evaluation of certain food additives. Prepared by the 51st meeting of the Joint FAO/WHO Expert Committee on Food Additives (JECFA), World Health Organization, Geneva, WHO Food Additives Series, 42, 403–414

  • WHO (2000) WHO concise international chemical assessment. Document vol.26. World Health Organization, Geneva

    Google Scholar 

  • Winkeler HD, Puttins U, Levsen K (1988) Organic compounds in rainwater. Vom Wasser 70:107–117, in German

    CAS  Google Scholar 

  • Wood R, Foster L, Damant A, Key P (2004) Analytical methods for food additives. CRC, Boca Raton

    Book  Google Scholar 

  • Xie YT, Chen P, Wei WZ (1999) Rapid analysis of preservatives in beverages by ion chromatography with series piezoelectric quartz crystal as detector. Microchem J 61:58–68

    Article  CAS  Google Scholar 

Download references

Acknowledgments

Authors are grateful to Mr. Bahman Ahmadzadeh for his generous consulting and assistance.

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Correspondence to Khalil Farhadi.

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Kokya, T.A., Farhadi, K. & Kalhori, A.A. Optimized Dispersive Liquid–Liquid Microextraction and Determination of Sorbic Acid and Benzoic Acid in Beverage Samples by Gas Chromatography. Food Anal. Methods 5, 351–358 (2012). https://doi.org/10.1007/s12161-011-9245-x

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