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A high-performance liquid chromatography–evaporative light scattering detection–based quantitative analytical method for polyvinyl alcohol in food supplements with pyrolysis–gas chromatography/mass spectrometry-based verification

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Abstract

Polyvinyl alcohol (PVOH) is extensively used in agricultural, pharmaceutical, textile, and food industries. A new high-performance liquid chromatography (HPLC) method with evaporative light scattering detection (ELSD) was developed for the quantitative analysis of PVOH products. Pyrolysis–gas chromatography/mass spectrometry (Py–GC/MS) was employed for method verification. The HPLC–ELSD method exhibited acceptable linearity (R2 > 0.99), with limits of detection and quantitation of 19.43 and 58.88 μg/mL, respectively. Accuracies of 91.16–102.30% were estimated based on recoveries of the intra- and inter-day tests of PVOH. Repeatability and intermediate precision (%RSD) of 1.23–4.45 and 2.18–6.95, respectively, were obtained. The presence of PVOH in the HPLC peaks was further verified using typical indicators of PVOH in Py–GC/MS analysis, such as acetaldehyde, 2,5-dihydrofuran, benzaldehyde, and crotonaldehyde. This novel HPLC method with Py–GC/MS-based verification can be successfully applied for analyzing PVOH in dietary supplement tablets.

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References

  • Antić VV, Antić MP, Kronimus A, Oing K, Schwarzbauer J. Quantitative determination of poly (vinylpyrrolidone) by continuous-flow off-line pyrolysis-GC/MS. Journal of Analytical and Applied Pyrolysis. 90: 93-99 (2011)

    Article  Google Scholar 

  • Clarot I, Chaimbault P, Hasdenteufel F, Netter P, Nicolas A. Determination of gentamicin sulfate and related compounds by high-performance liquid chromatography with evaporative light scattering detection. Journal of Chromatography A. 1031: 281-287 (2004)

    Article  CAS  Google Scholar 

  • Cleaver G. Analysis of modified polyvinyl alcohol by GPC viscometry using the Agilent 390-MDS multi detector suite. 5991–5838EN. Agilent application note (2015)

  • DeMerlis C, Schoneker D. Review of the oral toxicity of polyvinyl alcohol (PVA). Food and chemical Toxicology. 41: 319-326 (2003)

    Article  CAS  Google Scholar 

  • Dunn KD. Determination of polyvinyl alcohol in a poly (DL-lactide-co-glycolide) matrix by size exclusion chromatography using evaporative light scattering detection. Journal of Pharmaceutical and Biomedical Analysis. 25: 539-543 (2001)

    Article  CAS  Google Scholar 

  • EFSA. Statement on the request for a modification of the specification on solubility of the food additive polyvinyl alcohol (E 1203) in ethanol and its possible impact on the safety assessment. EFSA Journal. 12: 3820 (2014)

    Google Scholar 

  • European Parliament the Council of the European Union. Regulation (EC) No 1333/2008 of the European Parliament and of the Council of 16 December 2008 on food additives. Official Journal of the European Union. 354: 16-33 (2008)

    Google Scholar 

  • Food and Drug Administration. GRAS notice No. 141., U.S. FDA. GRAS Notice Inventory. https://www.cfsanappsexternal.fda.gov/scripts/fdcc/?set=GRASNotices&id=141&sort=GRN_No&order=DESC&startrow=1&type=basic&search=Polyvinyl%20alcohol. Accessed Feb 4, 2004.

  • Food and Drug Administration. Analytical procedures and methods validation for drugs and biologics–guidance for industry. https://www.fda.gov/regulatory-information/search-fda-guidance-documents/analytical-procedures-and-methods-validation-drugs-and-biologics. Accessed Jul 30, 2015

  • Food and Drug Administration. GRAS notice No. 767., U.S. FDA. GRAS Notice Inventory. https://www.fda.gov/media/128920/download. Accessed Feb 4, 2018

  • Fuh M-RS, Wang G-Y. Quantitative analysis of nitrile rubber/chloroprene by pyrolysis/gas chromatography/mass spectrometry. Analytica Chimica Acta. 371: 89-96 (1998)

    Article  CAS  Google Scholar 

  • Goodship V, Jacobs D. Polyvinyl alcohol: materials, processing and applications. Vol. 16. Smithers rapra technology (2009)

    Google Scholar 

  • ICH Harmonised Ttipartite, Guideline. Validation of analytical procedures: text and methodology. Q2 (R1), 1(20), 05 (2005)

  • Ishimura T, Iwai I, Matsui K, Mattonai M, Watanabe A, Robberson W, Cook A-M, Allen HL, Pipkin W, Teramae N. Qualitative and quantitative analysis of mixtures of microplastics in the presence of calcium carbonate by pyrolysis-GC/MS. Journal of Analytical and Applied Pyrolysis. 157: 105188 (2021)

    Article  CAS  Google Scholar 

  • JECFA. Chemical and Technical Assessment-Polyvinyl alcohol. 61st Joint FAO/WHO Expert Committee on Food Additives (2004)

    Google Scholar 

  • JECFA, Evaluation of certain food additives and contaminants: sixty-eighth report of the Joint FAO/WHO Expert Committee on Food Additives. World Health Organization. (2007).

    Google Scholar 

  • JECFA. Codex alimentarius, general standard for food additives (Adopted in 1995). (2019)

  • Jones S, Brown M, Martin G. Determination of polyvinyl alcohol using gel filtration liquid chromatography. Chromatographia. 59: 43-46 (2004)

    CAS  Google Scholar 

  • Kusch P. Introductory chapter: analytical pyrolysis-gas chromatography/mass spectrometry of polymeric materials. In: Analytical Pyrolysis. IntechOpen (2018)

    Google Scholar 

  • La Nasa J, Biale G, Fabbri D, Modugno F. A review on challenges and developments of analytical pyrolysis and other thermoanalytical techniques for the quali-quantitative determination of microplastics. Journal of Analytical and Applied Pyrolysis. 149: 104841 (2020)

    Article  Google Scholar 

  • Lai JCH, Rahman MR, Hamdan S, Liew FK, Rahman MM, Hossen MF. Impact of nanoclay on physicomechanical and thermal analysis of polyvinyl alcohol/fumed silica/clay nanocomposites. Journal of Applied Polymer Science. 132 (2015)

    Article  Google Scholar 

  • Ministry of Food and Drug Safety. Guidelines on performance criteria and validation of analytical methods for the detection of chemical/microbial factors in foods (2017)

  • Ministry of Food and Drug Safety. Food additives code. https://www.mfds.go.kr/eng/brd/m_15/view.do?seq=72242&srchFr=&srchTo=&srchWord=&srchTp=&itm_seq_1=0&itm_seq_2=0&multi_itm_seq=0&company_cd=&company_nm=&page=1. Accessed June 30, 2020

  • Moldoveanu S. Analytical pyrolysis of synthetic organic polymers. Elsevier (2005)

    Google Scholar 

  • Nagy DJ. Size exclusion chromatography of polyvinyl alcohol and polyvinyl acetate. Handbook Of Size Exclusion Chromatography And Related Techniques: Revised And Expanded 91: 269 (2003)

    Google Scholar 

  • National Health and Family Planning Commission. National food safety standard for uses of food additives GB 2760–2014. http://www.cirs-reach.com/Uploads/file/20180428/1524879613_22618.pdf. Accessed June 30, 2020

  • Procházková L, Rodríguez-Muñoz Y, Procházka J, Wanner J. Simple spectrophotometric method for determination of polyvinylalcohol in different types of wastewater. International Journal of Environmental Analytical Chemistry. 94: 399-410 (2014)

    Article  Google Scholar 

  • Shi R, Bi J, Zhang Z, Zhu A, Chen D, Zhou X, Zhang L, Tian W. The effect of citric acid on the structural properties and cytotoxicity of the polyvinyl alcohol/starch films when molding at high temperature. Carbohydrate Polymers. 74: 763-770 (2008)

    Article  CAS  Google Scholar 

  • Tsuge S, Ohtani H, Watanabe C. Pyrolysis-GC/MS data book of synthetic polymers: pyrograms, thermograms and MS of pyrolyzates. Elsevier (2011)

    Google Scholar 

  • Wasik A, McCourt J, Buchgraber M. Simultaneous determination of nine intense sweeteners in foodstuffs by high performance liquid chromatography and evaporative light scattering detection—development and single-laboratory validation. Journal of Chromatography A. 1157: 187-196 (2007)

    Article  CAS  Google Scholar 

  • WHO. Safety evaluation of certain food additives and contaminants. (2004)

    Google Scholar 

  • Zeynali M, Nazari M, Karimi S, Seyedmohaghegh S, Soltani S. Prediction of polyvinyl alcohol (PVOH) properties synthesized at various conditions by artificial neural networks technique. Iranian Journal of Chemical Engineering. 14: 3-16 (2017)

    Google Scholar 

Download references

Acknowledgements

This research was supported by a Grant (18162MFDS009) from the Ministry of Food and Drug Safety in 2018. This research was also supported by the Chung-Ang University Graduate Research Scholarship (Academic scholarship for College of Biotechnology and Natural Resources) in 2021.

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Authors and Affiliations

  1. Department of Food Science and Technology, Chung-Ang University, 4726, Seodong-daero, Anseong, Gyeonggi-do, 17546, Republic of Korea

    Juhee Park, Jihee Lee, Min ji Kang, Jihyun Lee, Hee-Seok Lee & Chan Lee

  2. Food Analysis Research Center, Korea Food Research Institute, Wanju, Jeollabuk-do, 55365, Republic of Korea

    Juhee Park

  3. Department of Environmental Engineering, Daegu University, Gyeongsan, 38543, Republic of Korea

    Young-Min Kim

  4. Department of Food Science, Sun Moon University, Asan, Chungchengnam-do, 31460, Republic of Korea

    Hee-Jae Suh

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  1. Juhee Park
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  3. Young-Min Kim
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  4. Min ji Kang
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Correspondence to Chan Lee.

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Park, J., Lee, J., Kim, YM. et al. A high-performance liquid chromatography–evaporative light scattering detection–based quantitative analytical method for polyvinyl alcohol in food supplements with pyrolysis–gas chromatography/mass spectrometry-based verification. Food Sci Biotechnol 31, 797–805 (2022). https://doi.org/10.1007/s10068-022-01102-2

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