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. 2016 Oct 31;25(5):1305–1311. doi: 10.1007/s10068-016-0205-5

Validation and measurement uncertainty evaluation of the GC-MS method for the direct determination of hexamethylenetetramine from foods

Ho Soo Lim 1,✉, Ju Young Hwang 1, Jung Im Kim 1, Jae Chon Choi 1, Meehye Kim 1
PMCID: PMC6049282  PMID: 30263409

Abstract

A simple GC-MS method has been developed and validated for the direct determination of hexamethylenetetramine (HMT). The separation of HMT was performed using a MXT-1 column. The calibration curve was linear over the concentration range 0.1-25 μg/mL, with a good correlation coefficient (r =0.9996). The recoveries of HMT from foods spiked at 1, 5, and 10 μg/g ranged from 91.7% to 115.2%. Intra-day (n=5) and inter-day (n=5) precision were less than 7%. The limit of detection and the limit of quantification of the method were 0.05 and 0.15 μg/mL, respectively. The uncertainties associated with food matrix and calibration contributed most to the overall expanded uncertainty. The method validation data indicated that quantitative method could be applied to the direct determination of non-hydrolyzed HMT in foods.

Keywords: hexamethylenetetramine, gas chromatography-mass spectrometry, direct determination, method validation

References

  • 1.Restani P, Corsini E, Galli CL. A novel approach to quantify the amount of formaldehyde added to milk in grana padano cheese production. J. Food Sci. 1989;54:578–580. doi: 10.1111/j.1365-2621.1989.tb04656.x. [DOI] [Google Scholar]
  • 2.European Commission. European Parliament and Council Directive No 95/2/EC on Food Additives other than Colors and Sweeteners. Off. J. Eur. Comm. L61: 1–40 (1995)
  • 3.Codex Alimentarius Commission. CODEX General Standard for Food Additives CODEX STAN 192-1995. Available from: http://www.codexalimentarius.net/gsfaonline/docs/CXS192e.pdf. Accessed Mar. 3, 2015.
  • 4.Korea Ministry of Food and Drug Safety. Korea Food Additives Code. Korea Food Industry Association, Seoul, Korea (2014)
  • 5.US Food and Drug Administration (FDA). Food Additive Listings. Available from: http://www.fda.gov/Food/IngredientsPackagingLabeling/FoodAdditives Ingredients. Accessed Mar. 3, 2015.
  • 6.Ministry of Health, Labor and Welfare. Food Additives. Available from: http://www.mhlw.go.jp/english/topics/foodsafety/foodadditives. Accessed Mar. 3, 2015.
  • 7.Joint FAO/WHO Expert Committee on Food Additives. Toxicological evaluation of certain food additives with a review of general principles and of specifications. WHO Technical Report Series No. 539. Available from: http://apps.who.int/food-additives-contaminants-jecfa-database/search.aspx. Accessed Mar. 3, 2015. [PubMed]
  • 8.World Health Organization (WHO). Formaldehyde. Environmental Health Criteria 89 (Geneva: WHO) (1989)
  • 9.Lim HS, Kim JI, Ko KY, Kim M. Determination of hexamethylenetetramine in foods by high-performance liquid chromatography (HPLC) Food Addit. Contam. A. 2014;31:1489–1495. doi: 10.1080/19440049.2014.942706. [DOI] [PubMed] [Google Scholar]
  • 10.Pavitrapok C, Williams DA. Determination of methenamine, methenamine mandelate and methenamine hippurate in pharmaceutical preparations using ion-exchange HPLC. J. Pharm. Biomed. Anal. 2006;40:1243–1248. doi: 10.1016/j.jpba.2005.09.017. [DOI] [PubMed] [Google Scholar]
  • 11.Koga M, Shinohara R, Akiyama T. Gas chromatographic determination of trace amounts of hexamethylenetetramine in water using an iodine charge-transfer complex. Anal. Sci. 1985;1:381–384. doi: 10.2116/analsci.1.381. [DOI] [Google Scholar]
  • 12.Cottin H, Szopa C, Moore MH. Production of hexamethylenetetramine in photolyzed and irradiated interstellar cometary ice analogs. Astrophys. J. 2001;561:139–142. doi: 10.1086/324575. [DOI] [Google Scholar]
  • 13.Association of Official Analytical Chemists. Guidelines for single laboratory validation of chemical methods for dietary supplements and botanicals. Available from: http://www.aoac.org/imis15_prod/AOAC_Docs/Standards Development/SLV_guidelines_DietarySupplements.pdf>Accessed Mar. 3, 2015.
  • 14.International Conference on Harmonization (ICH). ICH harmonised tripartite guideline, validation of analytical procedures: text and methodology Q2 (R1). Available from: http://www.ich.org. Accessed Mar. 3, 2015.
  • 15.International Organization for Standardization. Guide to the expression of uncertainty in measurement (GUM). Available from: http://www.bipm.org/utils/common/documents/jcgm/JCGM_100_2008_E.pdf. Accessed Mar. 3, 2015.
  • 16.EURACHEM/CITAC Guide. CG4: Quantifying Uncertainty in Analytical Measurement. Available from: http://eurachem2011.fc.ul.pt/pdf/QUAM 2012_DIS1.pdf. Accessed Mar. 3, 2015.
  • 17.Stein SE. An integrated method for spectrum extraction and compound identification from gas chromatography/mass spectrometry data. J. Am. Soc. Mass Spectr. 1999;10:770–781. doi: 10.1016/S1044-0305(99)00047-1. [DOI] [Google Scholar]
  • 18.McMaster MC. GC/MS: A practical user’s guide. 2nd ed. John Wiley & Son, Inc., Hoboken, NJ, USA. pp. 1-180 (2008)
  • 19.Strom JG, Jun HW. Separation and quantitation of methenamine in urine by ion-pair extraction. J. Pharm. Sci. 1986;75:416–420. doi: 10.1002/jps.2600750422. [DOI] [PubMed] [Google Scholar]
  • 20.Iwakami Y, Takzono M. Thermal decomposition of hexamethylene tetramine. B. Chem. Soc. Jpn. 1968;41:813–817. doi: 10.1246/bcsj.41.813. [DOI] [Google Scholar]

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