Gıda Örneklerindeki İndigo Karminin (E132) Dispersif Katı Faz Mikroekstraksiyon Yöntemiyle Önderiştirilmesi ve Ayrılması

Abstract

Bu çalışmada, Fe3O4@XAD-7 nanopartikülü kullanılarak spektrofotometrik analiz öncesinde bazı gıda örneklerindeki İndigo Karminin (E132) önderiştirilmesi ve ayrılması için bir mikroekstraksiyon tekniği geliştirilmiştir. Öncelikle geliştirilen yöntemin pH, Fe3O4@XAD-7 nanopartikül miktarı, desorpsiyon çözücüsü türü, vorteks süresi, numune hacmi gibi parametrelerinin optimum koşulları belirlenmiştir. Optimum koşullar altında elde edilen sonuçlar, geliştirilen katı faz mikroekstraksiyon yönteminin 8–250 μgL̀-1 konsantrasyon aralığında 0,999'luk bir korelasyon katsayısı (R2) ve 2,1 μgL-1'lik bir tayin sınırı ile iyi doğrusallığa sahip olduğu bulunmuştur. Yöntemin % bağıl standart sapması (% RSD) % 2,3 olarak bulunmuştur. Geliştirilen yöntemin zenginleştirme faktörü (EF) ve önderiştirme faktörü (PF) sırasıyla 85 ve 71 olarak hesaplanmıştır. Geliştirilen yöntem gerçek gıda örneklerine uygulanmış ve %98-105 aralığında yüksek gerikazanımlar elde edilmiştir.

Keywords

• Dispersif katı faz mikroekstraksiyon metodu
• önderiştirme
• spektrofotometrik analiz
• indigo karmin

Preconcentration and Seperation of Indigo Carmine (E132) in Food Samples by Dispersive Solid Phase Microextraction Method

Abstract

In this study, a microextraction technique was produced using Fe3O4@XAD-7 nanoparticle for the preconcentration and separation of Indigo Carmine (E132) in some food samples prior to spectrophotometric analysis. Firstly, optimum conditions of parameters of developed method such as pH, amount of Fe3O4@XAD-7 nanoparticle, type of desorption solvent, vortex time, sample volume were determined. Under the optimum conditions, the obtained results, developed solid phase microextraction method possessed excellent linearity with a correlation coefficient (R2) of 0.999 in the concentration range of 8–250 μgL̀-1 and detection limit are 2.1 μgL-1. Relative standard deviation % (RSD%) of the method was calculated as 2.3%. Enhancement factor (EF) and preconcentration factor (PF) of the developed method were calculated to be 85 and 71, respectively. The developed method was applied to real food samples and high recoveries were obtained in the range of 98-105%.

Keywords

• Dispersive solid phase microextraction method
• preconcentration
• spectrophotometric analysis
• indigo carmine

References

1. Al-Salem HS, Alharbi SN, Al-Goul ST, Katameshc NS, Abdel-Lateef MA. A sustainable methodology employing the extract of red dragon fruit peel as a fluorescence probe for detection of indigo carmine (E132) in food samples: evaluation of the method's greenness, whiteness, and blueness. RSC Adv 2024; 14(33): 24010-24018.
2. Kizil N, Erbilgin DE, Yola ML, Soylak M. An environmentally friendly hydrophobic deep eutectic solvent dispersive liquid liquid microextraction for spectrophotometric analysis of indigo carmine (E132). Opt Quantum Electron 2024; 56(3):341.
3. Altunay N. An optimization approach for fast, simple and accurate determination of indigo-carmine in food samples, Spectrochim. Acta A Mol. Biomol Spectrosc 2021; 257:119791.
4. EFSA, Follow-up of the re-evaluation of indigo carmine (E 132) as a food additive, EFSA J 2023; 21(7): 1-31.
5. Berzas NJJ, Rodríguez FJ, Villaseñor LMJ, Rodríguez F. N. Simultaneous spectrophotometric determination of tartrazine, patent blue V, and indigo carmine in commercial products by partial least squares and principal component regression methods. Talanta 1999; 48:895–903.
6. Floriano L, Ribeiro LC, Saibt N, Bandeira NMG, Prestes OD, Zanella R. Determination of six synthetic dyes in sports drinks by dispersive solid-phase extraction and HPLC-UV-Vis. J Braz Chem Soc 2018; 29(3):602–608.
7. Deroco PB, Medeiros RA, Rocha-Filho RC, Fatibello-Filho O. Selective and simultaneous determination of indigo carmine and allura red in candy samples at the nano-concentration range by flow injection analysis with multiple pulse amperometric detection. Food Chem 2017; 247: 66–72.
8. López-de-Alba PL, López-Martínez L, De-León-Rodríguez L. M. Simultaneous Determination of Synthetic Dyes Tartrazine, Allura Red and Sunset Yellow by Differential Pulse Polarography and Partial Least Squares. A Multivariate Calibration Method. Electroanalysis 2002; 14(3): 197–205.

9. Korkmaz M. Central composite experimental design for Indigo Carmine dye removal from solutions by applying electrocoagulation and electrooxidation processes. Environ Res Tec 2025; 8(2): 382-398.
10. Waly SM, El-Wakil AM, Waly MM, Abou El-Maaty WM, Awad FS. Enhanced removal of indigo carmine dye from aqueous solutions using polyaniline modified partially reduced graphene oxide composite. Sci Rep 2025; 15: 15555.
11. Reyes-Garcés N, Gionfriddo E, Gómez-Ríos AG, Alam N, Boyacı E, Bojko B, Singh V, Grandy J, Pawliszyn J. Advances in Solid Phase Microextraction and Perspective on Future Directions. Anal Chem 2018; 90(1): 302−360.
12. Khan WA, Varanusupakul P, Ul Haq H, Arain MB, Boczkaj G. Applications of nanosorbents in dispersive solid phase extraction/microextraction approaches for monitoring of synthetic dyes in various types of samples: A review. Microchem J 2025; 208; 112419.
13. Chang-Hua X, Guo-Sheng C, Zhen-Hai X, Yu-Xia F, Xi Chang W, Yuan L. Applications of solid-phase microextraction in food analysis. TrAC 2016; 80: 12-29.
14. Ghorbani M, Aghamohammadhassan M, Chamsaz M, Akhlagh H, Pedramrad T. Dispersive solid phase microextraction. TrAC 2019; 118(1):793-809.
15. Erek F, Lanjwani MF, Tuzen M. A sensitive determination of Brilliant Blue FCF in some food samples using hydrophillic deep eutectic solvent-assisted magnetic nano gel-based dispersive solid phase microextraction prior to spectrophotometric analysis. Food Chem 2024; 453:139632.
16. Tong Y, Zhou Q, Sun Y, Sheng X, Zhou B, Zhao J, Guo J. Magnetic polyamidoamine dendrimer grafted with 4-mercaptobenzoic acid as an adsorbent for preconcentration and sensitive determination of polycyclic aromatic hydrocarbons from environmental water samples. Talanta 2021; 224: 121884.
17. Arain MB, Niaz A, Soylak M. Dispersive solid-phase microextraction of Cd(II) using CaFe layer double hydroxide with g-C3N4 nanocomposite from food and environmental samples. Food Chem 2025; 476:143410
18. Turkish Food Codex Regulation, Communication on Colorants Used in Food. (2008). URL: https://www.resmigazete.gov.tr/eskiler/2008/05/20080522-7.htm, (07.12.2024).
19. Üstün ÖM, Delmidan M. Development and validation of an effective spectrophotometric method for simultaneous determination of synthetic colorants after cloud point extraction and comparision with new green HPLC method. J AOAC Int 2019; 102(4):1241–1252.
20. Gharaghani FM, Akhond M, Hemmateenejad B. A three-dimensional origami microfluidic device for paper chromatography: Application to quantification of Tartrazine and Indigo carmine in food samples. J Chromatogr A 2020;1621: 461049.