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Detection of Methyl Orange in Saffron and Other Edibles Using Direct Injection Micellar Liquid Chromatography

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Abstract

A simple, sensitive, rapid and eco friendly micellar liquid chromatographic method was developed for the detection of banned color methyl orange in counterfeit saffron and prepared foodstuffs. Methyl orange (p-[[p-(dimethylamino) phenyl] azo] benzenesulfonic acid sodium salt) is a hazardous dye used in titration and is known to be used as common adulterant in counterfeit saffron and cooked foodstuffs like Jalebi (Indian sweet), mango shake, Namkeen (salted snacks), tomato ketchup and ice candy etc., due to its pleasant orange color. In the present work, methyl orange was detected in various food samples using direct injection micellar liquid chromatography without any pretreatment step. A C18 column with an optimum micellar mobile phase containing 0.05-M sodium dodecyl sulfate (SDS), 2 % pentanol buffered to pH 7 was used. Detection was carried out at 458 nm. The retention time was 3.7 min without showing any matrix effect. Linearity (r > 0.9999), intraday and interday precision RSD (%) was less than 1.00 in micellar media. Limit of detection and quantification was found to be 0.05 mg/kg and 0.10 mg/kg, respectively. Robustness study was also included as a part of method validation. The developed method proved to be reliable and sensitive for determination of methyl orange in real food samples.

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References

  • Agrawal N, Peiro SM, Romero JE, Durgbanshi A, Bose D, Vicente JP, Broch SC (2014) Determination of paroxetine in blood and urine using micellar liquid chromatography with electrochemical detection. J Chromatogr Sci 20:1–7

    Google Scholar 

  • Ashok V, Agrawal N, Durgbanshi A, Romero JE, Bose D (2014) Determination of adulteration of malachite green in green pea and some prepared foodstuffs by micellar liquid chromatography. J AOAC Inter 97:1387–1392

    Article  CAS  Google Scholar 

  • Ashok V, Agrawal N, Durgbanshi A, Romero JE, Bose D (2015) A novel micellar chromatographic procedure for the determination of metanil yellow in foodstuffs. Anal Methods 7:9324–9330

    Article  CAS  Google Scholar 

  • Berthod A, Alvarez CG (2000) In: Cazes J (ed) Micellar liquid chromatography. Marcel-Dekker, New York

    Google Scholar 

  • Bose D, Durgbanshi A, Dominguez AM, Capella Peiro ME, Broch SC, Romero JE (2005) Rapid determination of acetaminophen in physiological fluids by liquid chromatography using SDS mobile phase and ED detection. J Chromatogr Sci 43:313–318

    Article  CAS  Google Scholar 

  • Botek P, Poustka J, Hajslova J (2007) Determination of banned dyes in spices by liquid chromatography mass spectrometry. Czech J Food Sci 25:17–24

    CAS  Google Scholar 

  • Branen AL, Davidson PM, Salminen S (1989) Food Additive. Marcel Dekker Inc, New York, pp 139–193

    Google Scholar 

  • Chemical land (2014) Methyl Orange. http://chemicalland21.com/specialty chem/finechem/ methylorange.html Accessed 08 November 2014

  • Djozan D, Karimian G, Jouyban GA, Iranmanesh F, Gorbanpour H, Akbar A (2014) Discrimination of saffron based on thin-layer chromatography and image analysis. J Planer Chromatogr 4:274–280

    Article  Google Scholar 

  • Elsalamony RA, Ghoneim SA (2013) Tio2 anatase nano-powder prepared by a gamma ray irradiation and photocatalytic activity. 2nd International Conference on Energy Systems and Technologies; Cairo, Egypt

  • Ertas E, Ozer H, Alasalvar C (2007) A rapid HPLC method for determination of sudan dyes and para red in red chili pepper. Food Chem 105:756–760

    Article  CAS  Google Scholar 

  • Esfanjani AF, Jafari SM, Assadppor E, Mohannadi A (2015) Nano-encapsulation of saffron extract through double-layered multiple emulsions of pectin and whey protein concentrate. J Food Enging 165:149–155

    Article  CAS  Google Scholar 

  • Falcon MS, Gandara SJ (2005) Determination of food dyes in soft drinks containing natural pigments by liquid chromatography with minimal cleanup. Food Control 16:293–297

    Article  Google Scholar 

  • Gonzalez M, Gallego M, Valcarcel M (2003) Determination of natural and synthetic colorants in prescreened dairy samples using liquid chromatography-diode array detection. J Anal Chem 75:685–693

    Article  CAS  Google Scholar 

  • Harp BP, Bermudez EM, Baron CI, Richard GI (2012) Qualitative identification of permitted and non-permitted colour additives in food products. Food Addit Contam Part A 29:886–896

    Article  CAS  Google Scholar 

  • Ishikawa F (2007) Analysis of food dyes in food: confirmation of the presence of non permitted dyes by LC-MS and structural analysis of unknown dyes by NMR. Foods Food Ingred J Jpn 212:968–976

    CAS  Google Scholar 

  • Khazaei KM, Jafari SM, Ghorbani M, Kakhki AM (2014) Application of maltodextrin and gum Arabic in microencapsulation of saffron petal’s anthocyanins and evaluating their storage stability and color. Carbohydr Polym 105:57–62

    Article  Google Scholar 

  • Khazaei KM, Jafari SM, Ghorbani M, Kakhki AM (2016) Optimization of anthocyanin extraction from saffron petals with response surface methodology. Food Anal Meth 15:1–9

    Google Scholar 

  • Kiseleva MG, Pimenova VV, Eller KI (2003) Optimization of conditions for the HPLC determination of synthetic dyes in food. J Anal Chem 58:685–690

    Article  CAS  Google Scholar 

  • Kobra H, Mohtasebi SS, Foroughirad A, Varnamkhasti MG, Rafiee S, Rezei K (2015) Detection of adulteration in saffron samples using electronic nose. Int J Food Prop 7:1391–1401

    Google Scholar 

  • Manual of methods of analysis of food additives, Lab manual 8 (2005a) Directorate General of Health Services. Ministry of Health and Family Welfare, New Delhi, India, pp 75–75

    Google Scholar 

  • Manual of methods of analysis of food additives, Lab manual 8 (2005b) Directorate General of Health Services. Ministry of Health and Family Welfare, New Delhi, India, pp 86–93

    Google Scholar 

  • Mehrnia MA, Jafari SM, Zadeh M, Maghsoudlou Y (2016) Crocin loaded nano-emulsions: factors affecting emulsion properties in spontaneous emulsification. Intern J Bio Macro 84:261–267

    Article  CAS  Google Scholar 

  • Minioti KS, Sakellariou CF, Thomaidis NS (2007) Determination of 13 synthetic food colorants in water-soluble foods by reversed-phase high-performance liquid chromatography coupled with diode-array detector. Anal Chim Acta 583:103–110

    Article  CAS  Google Scholar 

  • Mohammad I, Shukla SK, Shakeel W (2015) Rapid detection of adulteration in indigenous saffron of Kashmir Valley. India Res J Forensic Sci 3:07–11

    Google Scholar 

  • Rajabi H, Ghorbani M, Jafari SM, Rajabjadeh G (2015) Retention of saffron bioactive components by spray drying encapsulation using maltodextrin, gum Arabic and gelatin as wall materials. Food hydrol 51:327–337

    Article  CAS  Google Scholar 

  • Sabinto L, Scordino M, Gargano M, Bellingo A, Traulo P (2011) HPLC/PDA/ESI-MS evaluation of saffron (Crocus sativus L.) adulteration. Nat Prod Comm 6:1873–1876

    Google Scholar 

  • Sarfarazi M, Jafari SM, Rajabzadeh G (2015) Extraction optimization of saffron nutraceuticals through response surface methodology. Food Anal Meth 9:2273–2285

    Article  Google Scholar 

  • Sforza S (2012) Food Authentication using bioorganic molecules. Destech Publications Inc. Lancaster, Pennsylvania, USA, pp 312–312

    Google Scholar 

  • Shukla SK, Iqbal M (2015) Forensic analysis of the saffron: rapid authenticity testing. Int J Rese Appl Sci Eng Technol 3:139–143

    Google Scholar 

  • Spectrum Chemical (2014) Methyl Orange Data Sheet http://www.spectrumchemical.com/ msds/m3970.pdf Accessed 04 November 2014

  • Wikipedia (2010) Methyl Orange. http://en.wikipedia.org/wiki/Methyl_orange.html Accessed 18 August 2014.

  • Yoshioka N, Ichihashi K (2007) Determination of 40 synthetic food colors in drinks and candies by high-performance liquid chromatography using a short column with photodiode array detection. Talanta 74:1408–1413

    Article  Google Scholar 

Download references

Acknowledgments

Vipin Ashok is thankful to the University Grants Commission (MHRD), Government of India, for awarding Rajiv Gandhi National Research Fellowship. The work was carried out as a joint venture between Dept. of Bioanalytical Chemistry, Universitat Jaume I, Castello, Spain and Dept. of Criminology & Forensic Science, Dr. Harisingh Gour University, Sagar (M.P.), India.

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Correspondence to Vipin Ashok.

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Vipin Ashok declares that he has no conflict of interest. Nitasha Agrawal declares that she has no conflict of interest. Josep Esteve-Romero declares that he has no conflict of interest. Devasish Bose declares that she has no conflict of interest. Neeti Prakash Dubey declares that he has no conflict of interest.

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Ashok, V., Agrawal, N., Esteve-Romero, J. et al. Detection of Methyl Orange in Saffron and Other Edibles Using Direct Injection Micellar Liquid Chromatography. Food Anal. Methods 10, 269–276 (2017). https://doi.org/10.1007/s12161-016-0578-3

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  • DOI: https://doi.org/10.1007/s12161-016-0578-3

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