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A Fast and Simple Method for Determination of Vitamin E in Infant Formula by Dispersive Liquid-Liquid Microextraction Combined with HPLC-UV

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Abstract

Developing a simple and fast method for quantification of vitamins in complex matrixes is one of the important issues in quality control of foods such as milk. In this study, after introducing a new method for quantification of vitamin E in infant formula, its content was compared to the label claims. In this study, dispersive liquid-liquid microextraction (DLLME) procedure with acetonitrile and chloroform as dispersive and extraction solvents, respectively, was used for isolation and clean-up of vitamin E from infant formula samples without the need for saponification. Then, reversed-phase high-performance liquid chromatography (RP-HPLC) composed of a C18 column as stationary phase and the mixture of acetonitrile, methanol, and water (91:8:1%) as mobile phase using a standard addition method was employed for quantification of vitamin E (α-tocopheryl acetate) with UV detection at 296 nm. After method validation under the optimum conditions, the method provided a linear range with a determination coefficient (R2) of 0.99 and acceptable accuracy and precision. Results showed that the developed method is an appropriate method for quality control of infant formulas. The advantage of DLLME compared with saponification process and liquid-liquid extraction is the decrease of organic solvent consumption and proposing of a simple and fast method for analysis of vitamin E in infant formula. Application of the developed method for analysis of vitamin E in infant formulas on the market showed there was a considerable difference between labeled and obtained content in most of the samples.

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References

  • Ababio PF, Adi DD, Amoah M (2012) Evaluating the awareness and importance of food labelling information among consumers in the Kumasi metropolis of Ghana. Food Control 26:571–574

    Article  Google Scholar 

  • Ake M, Fabre H, Malan AK, Mandrou B (1998) Column liquid chromatography determination of vitamins A and E in powdered milk and local flour: a validation procedure. J Chromatogr A 826:183–189

    Article  CAS  PubMed  Google Scholar 

  • Alshana U, Göğer NG, Ertaş N (2013) Dispersive liquid–liquid microextraction combined with field-amplified sample stacking in capillary electrophoresis for the determination of non-steroidal anti-inflammatory drugs in milk and dairy products. Food Chem 38:890–897

    Article  CAS  Google Scholar 

  • Alshana U, Ertaş N, Göğer NG (2015) Determination of parabens in human milk and other food samples by capillary electrophoresis after dispersive liquid–liquid microextraction with back-extraction. Food Chem 181:1–8

    Article  CAS  PubMed  Google Scholar 

  • Altunay N, Gürkan R (2016) Simultaneous determination of antimony and boron in beverage and dairy products by flame atomic absorption spectrometry after separation and preconcentration by cloud-point extraction. Food Addit Contam Part A Chem Anal Control Expo Risk Assess 33:271–281

    CAS  PubMed  Google Scholar 

  • Amoli-Diva M, Taherimaslak Z, Allahyari M, Pourghazi K, Manafi MH (2015) Application of dispersive liquid–liquid microextraction coupled with vortex-assisted hydrophobic magnetic nanoparticles based solid-phase extraction for determination of aflatoxin M1 in milk samples by sensitive micelle enhanced spectrofluorimetry. Talanta 134:98–104

    Article  CAS  PubMed  Google Scholar 

  • Barba FJ, Esteve MJ, Frígola A (2011) Determination of vitamins E (α-, γ- and δ-tocopherol) and D (cholecalciferol and ergocalciferol) by liquid chromatography in milk, fruit juice and vegetable beverage. Eur Food Res Technol 232:829–836

    Article  CAS  Google Scholar 

  • Berger TA, Berger BK (2013) Separation of 9 sulfonamide drugs in ≈ 4 min by ultra-high performance supercritical fluid chromatography (UHPSFC): with a feasibility study for detection in milk. Chromatographia 76:1631–1639

    Article  CAS  Google Scholar 

  • Cannoosamy K, Jeewon R (2016) A critical assessment of nutrition labelling and determinants of its use and understanding. Prog Nutr 18:195–204

    Google Scholar 

  • Carro A, González P, Lorenzo R (2013) Simultaneous derivatization and ultrasound-assisted dispersive liquid–liquid microextraction of chloropropanols in soy milk and other aqueous matrices combined with gas-chromatography–mass spectrometry. J Chromatogr A 1319:35–45

    Article  CAS  PubMed  Google Scholar 

  • Chávez-Servín JL, Castellote AI, López-Sabater MC (2006) Simultaneous analysis of vitamins A and E in infant milk-based formulae by normal-phase high-performance liquid chromatography–diode array detection using a short narrow-bore column. J Chromatogr A 1122:138–143

    Article  CAS  PubMed  Google Scholar 

  • Chotyakul N, Pateiro-Moure M, Saraiva JA, Torres JA, Pérez-Lamela C (2014) Simultaneous HPLC–DAD quantification of vitamins A and E content in raw, pasteurized, and UHT cow’s milk and their changes during storage. Eur Food Res Technol 238:535–547

    Article  CAS  Google Scholar 

  • Davies P, Funder J, Palmer D, Sinn J, Vickers M, Wall C (2016) Early life nutrition and the opportunity to influence long-term health: an Australasian perspective. J Dev Orig Health Dis 7:440–448

    Article  CAS  PubMed  Google Scholar 

  • Fanali C, D'Orazio G, Fanali S, Gentili A (2017) Advanced analytical techniques for fat-soluble vitamin analysis. Trends Anal Chem 87:82–97

    Article  CAS  Google Scholar 

  • Farajbakhsh F, Amjadi M, Manzoori J, Ardalan MR, Jouyban A (2016) Microextraction methods for preconcentration of aluminium in urine samples. Pharm Sci 22:87–95

    Article  Google Scholar 

  • Faraji M, Adeli M (2017) Sensitive determination of melamine in milk and powdered infant formula samples by high-performance liquid chromatography using dabsyl chloride derivatization followed by dispersive liquid–liquid microextraction. Food Chem 221:139–146

    Article  CAS  PubMed  Google Scholar 

  • Faraji M, Noorani M, Sahneh BN (2017) Quick, easy, cheap, effective, rugged, and safe method followed by ionic liquid-dispersive liquid–liquid microextraction for the determination of trace amount of bisphenol A in canned foods. Food Anal Methods 10:764–772

    Article  Google Scholar 

  • Gentili A, Caretti F, Bellante S, Ventura S, Canepari S, Curini R (2012) Comprehensive profiling of carotenoids and fat-soluble vitamins in milk from different animal species by LC-DAD-MS/MS hyphenation. J Agric Food Chem 61:1628–1639

    Article  CAS  PubMed  Google Scholar 

  • Giam C, Wong M (1987) Plasticizers in food. J Food Prot 50:769–782

    Article  CAS  PubMed  Google Scholar 

  • He L, Rodda T, Haynes CL, Deschaines T, Strother T, Diez-Gonzalez F, Labuza TP (2011) Detection of a foreign protein in milk using surface-enhanced Raman spectroscopy coupled with antibody-modified silver dendrites. Anal Chem 83:1510–1513

    Article  CAS  PubMed  Google Scholar 

  • Herrera-Herrera AV, Asensio-Ramos M, Hernández-Borges J, Rodríguez-Delgado MÁ (2010) Dispersive liquid-liquid microextraction for determination of organic analytes. Trends Anal Chem 29:728–751

    Article  CAS  Google Scholar 

  • Ishizaki A, Saito K, Hanioka N, Narimatsu S, Kataoka H (2010) Determination of polycyclic aromatic hydrocarbons in food samples by automated on-line in-tube solid-phase microextraction coupled with high-performance liquid chromatography-fluorescence detection. J Chromatogr A 1217:5555–5563

    Article  CAS  PubMed  Google Scholar 

  • Karami-Osboo R, Miri R, Javidnia K, Kobarfard F (2016) Simultaneous chloramphenicol and florfenicol determination by a validated DLLME-HPLC-UV method in pasteurized milk. Iran J Pharm Res 15(3):361–368

    CAS  PubMed  PubMed Central  Google Scholar 

  • Lennox A, Sommerville J, Ong K, Henderson H, Allen R (2013) Diet and nutrition survey of infants and young children, 2011. A survey carried out on behalf of the Department of Health and Food Standards Agency

  • Liu S, Xie Q, Cao J, Song P, Chen J, Bai W (2013) Rapid determination of α-tocopherol in cereal grains using dispersive liquid–liquid microextraction followed by HPLC. J Sep Sci 36:1135–1141

    Article  CAS  PubMed  Google Scholar 

  • Loughrill E, Govinden P, Zand N (2016) Vitamins A and E content of commercial infant foods in the UK: a cause for concern? Food Chem 210:56–62

    Article  CAS  PubMed  Google Scholar 

  • Mahan LK, Raymond JL (2016) Krause’s food & the nutrition care process. Elsevier, Amestrdam

    Google Scholar 

  • Mahmoudpour M, Mohtadinia J, Ansarin M, Nemati M (2016) Dispersive liquid–liquid microextraction for HPLC-UV determination of PAHs in milk. J AOAC Int 99:527–533

    Article  CAS  PubMed  Google Scholar 

  • Mahmoudpour M, Mohtadinia J, Mousavi MM, Ansarin M, Nemati M (2017) Application of the microwave-assisted extraction and dispersive liquid–liquid microextraction for the analysis of PAHs in smoked rice. Food Anal Methods 10:277–286

    Article  Google Scholar 

  • McMahon A, Christiansen S, Shine L, Loi C, Dowell D (2013) Simultaneous determination of 13-cis and all-trans vitamin a palmitate (retinyl palmitate), vitamin a acetate (retinyl acetate), and total vitamin E (α-tocopherol and dl-α-tocopherol acetate) in infant formula and adult nutritionals by normal phase HPLC: first action 2012.10. J AOAC Int 96:1073–1081

    Article  CAS  PubMed  Google Scholar 

  • Mohamed R, Richoz PJ, Gremaud E, Mottier P, Yilmaz E, Tabet JC, Guy PA (2007) Advantages of molecularly imprinted polymers LC-ESI-MS/MS for the selective extraction and quantification of chloramphenicol in milk-based matrixes. Comparison with a classical sample preparation. Anal Chem 79:9557–9565

    Article  CAS  PubMed  Google Scholar 

  • Mousavi MM, Nemati M, Alizadeh Nabili AA, Mahmoudpour M, Arefhosseini S (2016) Application of dispersive liquid–liquid microextraction followed by gas chromatography/mass spectrometry as effective tool for trace analysis of organochlorine pesticide residues in honey samples. J Iran Chem Soc 13:2211–2218

    Article  CAS  Google Scholar 

  • Nielsen SS (2010) Food analysis. Springer, New York

    Book  Google Scholar 

  • Nimalaratne C, Sun C, Wu J, Curtis JM, Schieber A (2014) Quantification of selected fat soluble vitamins and carotenoids in infant formula and dietary supplements using fast liquid chromatography coupled with tandem mass spectrometry. Food Res Int 66:69–77

    Article  CAS  Google Scholar 

  • Ozkan SA (2018) Analytical method validation: the importance for pharmaceutical analysis. Pharm Sci 24:1–2

    Article  Google Scholar 

  • Padró JM, Pellegrino Vidal RB, Echevarria RN, Califano AN, Reta MR (2015) Development of an ionic-liquid-based dispersive liquid–liquid microextraction method for the determination of antichagasic drugs in human breast milk: optimization by central composite design. J Sep Sci 38:1591–1600

    Article  CAS  PubMed  Google Scholar 

  • Phillips MM, Sharpless KE, Wise SA (2013) Standard reference materials for food analysis. Anal Bioanal Chem 405:4325–4335

    Article  CAS  PubMed  Google Scholar 

  • Plozza T, Trenerry VC, Caridi D (2012) The simultaneous determination of vitamins A, E and β-carotene in bovine milk by high performance liquid chromatography–ion trap mass spectrometry (HPLC–MSn). Food Chem 134:559–563

    Article  CAS  Google Scholar 

  • Quigley A, Cummins W, Connolly D (2016) Dispersive liquid-liquid microextraction in the analysis of milk and dairy products: a review. J Chem 2016:4040165

    Article  CAS  Google Scholar 

  • Rezaee M, Assadi Y, Hosseini M-RM, 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 

  • Ritota M, Manzi P (2018) Melamine detection in milk and dairy products: traditional analytical methods and recent developments. Food Anal Methods 11:128–147

    Article  Google Scholar 

  • Roe M, Pinchen H, Church S, Finglas P (2015) McCance and Widdowson’s the composition of foods seventh summary edition and updated composition of foods integrated dataset. Nutr Bull 40:36–39

    Article  Google Scholar 

  • Ross C, Caballero B, Cousins RJ, Tucker KL, Ziegler TR (2014) Modern nutrition in health and disease. Lippincott Williams & Wilkins, Philadelphia

    Google Scholar 

  • Rusnáková L, Andruch V, Balogh IS, Škrlíková J (2011) A dispersive liquid–liquid microextraction procedure for determination of boron in water after ultrasound-assisted conversion to tetrafluoroborate. Talanta 85:541–545

    Article  CAS  PubMed  Google Scholar 

  • Shammugasamy B, Ramakrishnan Y, Ghazali HM, Muhammad K (2013) Combination of saponification and dispersive liquid–liquid microextraction for the determination of tocopherols and tocotrienols in cereals by reversed-phase high-performance liquid chromatography. J Chromatogr A 1300:31–37

    Article  CAS  PubMed  Google Scholar 

  • Shehata AB, Rizk MS, Farag AM, Tahoun IF (2015) Development of two reference materials for all trans-retinol, retinyl palmitate, α-and γ-tocopherol in milk powder and infant formula. J Food Drug Anal 23:82–92

    Article  CAS  PubMed  Google Scholar 

  • Sunarić S, Živković J, Pavlović R, Kocić G, Trutić N, Živanović S (2012) Assessment of α-tocopherol content in cow and goat milk from the Serbian market. Hemijska Industrija 66:559–566

    Article  CAS  Google Scholar 

  • Sunarić S, Lalić J, Spasić A (2017) Simultaneous determination of alpha-tocopherol and alpha-tocopheryl acetate in dairy products, plant milks and health supplements by using SPE and HPLC method. Food Anal Methods 10:3886–3901

    Article  Google Scholar 

  • Ulusoy S, Acidereli H, Erdoǧan S, Ulusoy HI (2016) A new approach to the determination of folic acid at trace levels: using a Fe(III)-folic acid complex to amplify analytical signal. RSC Adv 6:40115–40122

    Article  CAS  Google Scholar 

  • Ulusoy HI, Acidereli H, Tutar U (2017a) Optimization of extraction parameters for fat soluble vitamins and major element analysis in Polygonum cognatum Meissn plant (Madimak). J Turkish Chem Soc Sect Chem 4:165–178

    Article  CAS  Google Scholar 

  • Ulusoy HI, Acidereli H, Ulusoy S, Erdoğan S (2017b) Development of a new methodology for determination of vitamin B9 at trace levels by ultrasonic-assisted cloud point extraction prior to HPLC. Food Anal Methods 10:799–808

    Article  Google Scholar 

  • Viñas P, López-García I, Bravo-Bravo M, Briceño M, Hernández-Córdoba M (2012) Dispersive liquid–liquid microextraction coupled to liquid chromatography for thiamine determination in foods. Anal Bioanal Chem 403:1059–1066

    Article  CAS  PubMed  Google Scholar 

  • Viñas P, Bravo-Bravo M, López-García I, Pastor-Belda M, Hernández-Córdoba M (2014a) Pressurized liquid extraction and dispersive liquid–liquid microextraction for determination of tocopherols and tocotrienols in plant foods by liquid chromatography with fluorescence and atmospheric pressure chemical ionization-mass spectrometry detection. Talanta 119:98–104

    Article  CAS  PubMed  Google Scholar 

  • Viñas P, Pastor-Belda M, Campillo N, Bravo-Bravo M, Hernández-Córdoba M (2014b) Capillary liquid chromatography combined with pressurized liquid extraction and dispersive liquid–liquid microextraction for the determination of vitamin E in cosmetic products. J Pharm Biomed Anal 94:173–179

    Article  CAS  PubMed  Google Scholar 

  • Woollard DC, Bensch A, Indyk H, McMahon A (2016) Determination of vitamin A and vitamin E esters in infant formulae and fortified milk powders by HPLC: use of internal standardisation. Food Chem 197:457–465

    Article  CAS  PubMed  Google Scholar 

  • Xie Q, Liu S, Fan Y, Zhang X (2014) Development of a dispersive liquid–liquid microextraction method for the determination of α-tocopherol in pigmented wheat by high-performance liquid chromatography. Food Anal Methods 7:21–30

    Article  Google Scholar 

  • Yan H, Cheng X, Liu B (2011) Simultaneous determination of six phthalate esters in bottled milks using ultrasound-assisted dispersive liquid–liquid microextraction coupled with gas chromatography. J Chromatogr B 879:2507–2512

    Article  CAS  Google Scholar 

  • Yazdi AS, Yazdinezhad SR (2014) Simultaneous determination of vitamin A and E in infant milk formulas using semi-micro liquid–liquid extraction followed by HPLC-UV. J Liq Chromatogr Relat Technol 37:391–403

    Article  CAS  Google Scholar 

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Funding

This study was funded by the Vice Chancellor for Research of Tabriz University of Medical Sciences, Tabriz, Iran, for a partial financial support, and it is a part of F. Sardikia’s M.S. thesis (No. 10) registered at Faculty of Pharmacy, Tabriz University of Medical Sciences, Tabriz, Iran.

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Authors and Affiliations

  1. Food and Drug Safety Research Center, Tabriz University of Medical Sciences, Tabriz, Iran

    Fatemeh Sadrykia

  2. Student Research Committee, Tabriz University of Medical Sciences, Tabriz, Iran

    Fatemeh Sadrykia

  3. Pharmaceutical Analysis Research Center, Tabriz University of Medical Sciences, Tabriz, Iran

    Ali Shayanfar

  4. Drug Applied Research Center, Tabriz University of Medical Sciences, Tabriz, Iran

    Hadi Valizadeh

  5. Halal Research Center of IRI, FDA, Tehran, Iran

    Mahboob Nemati

  6. Faculty of Pharmacy, Tabriz University of Medical Sciences, Tabriz, Iran

    Mahboob Nemati

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  1. Fatemeh Sadrykia
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  2. Ali Shayanfar
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  3. Hadi Valizadeh
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  4. Mahboob Nemati
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Correspondence to Mahboob Nemati.

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Fatemeh Sadrykia declares that she has no conflict of interest. Ali Shayanfar declares that he has no conflict of interest. Hadi Valizadeh declares that he has no conflict of interest. Mahboob Nemati declares that he has no conflict of interest.

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Sadrykia, F., Shayanfar, A., Valizadeh, H. et al. A Fast and Simple Method for Determination of Vitamin E in Infant Formula by Dispersive Liquid-Liquid Microextraction Combined with HPLC-UV. Food Anal. Methods 12, 23–31 (2019). https://doi.org/10.1007/s12161-018-1331-x

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