• LAKSHMI NARASIMHA RAO KATAKAM Department of Analytical Development, Saptalis Pharmaceuticals LLC, Hauppauge, New York 11788, USA.
  • THIRUPATHI DONGALA Department of Analytical Research and Development, Aurex Laboratories LLC, New Jersey 08520, USA.



1,4-Dioxane, Sodium laureth sulfate, Raw material, Gas chromatographic with flame ionization detection, Trace level determination


Objective: The study spotlights on a new gas chromatographic (GC) method with flame ionization detection technique that has been developed and validated for the selective determination of 1,4-dioxane content in sodium laureth sulfate (SLS), raw material.

Methods: The method was developed using a Thermo Scientific TR-1 (30 m×0.25 mm×1.0 μm) column with a carrier gas used as helium. The diluent used as purified water and the flow pressure of the carrier gas is 9.0 psi with a split ratio of 1:5. The optimized method was validated as per the ICH Q2 guidelines.

Results: Regression analysis confers a correlation coefficient for the stated compounds that are found to be greater than 0.999. The limit of quantitation and limit of detection are established at a sensitive determination level of 9 ppm and 3 ppm, respectively.

Conclusion: The validated and rugged GC method developed for the determination of 1,4-dioxane using a specific GC method in the SLS raw material. The recovery results prove the sound judgment in the determination of accuracy toward its evaluation. Hence, the validated analytical method was specific, selective, economical, and accurate for the determination of 1,4-dioxane by gas chromatographic method with flame ionization detection technique.


Download data is not yet available.


Tay BY, Maurad Z, Muhammad H. Gas chromatography with flame ionization detection of 1,4-dioxane in palm-based fatty alcohol ethoxylates. J Am Oil Chem Soc 2014;91:1103-10.

Scalia S. Reversed-phase high-performance liquid chromatographic method for the assay of 1,4-dioxane in sulphatedpolyoxyethylene alcohol surfactants. J Pharm Biomed Anal 1990;8:867-70.

Birkel TJ, Warner CR, Fazio T. Gas chromatographic determination of 1,4-dioxane in polysorbate 60 and polysorbate 80. J Assoc Off Anal Chem 1979;62:931-6.

Robinson JJ, Ciurxczak EW. Direct gas chromatographic determination of 1,4-dioxane in ethoxylated surfactants. J Soc CosmetChem 1980;31:329-37.

Stafford ML, Guin KF, Johnson GA, Sanders LA, Rockey SL. Analysis of 1,4-dioxane in ethoxylated surfactants. J Soc CosmetChem 1980;31:281-7.

Waldman BA. Analysis of 1,4-dioxane in ethoxylated compounds by gas chromatography/mass spectrometry using selected ion monitoring.J Soc CosmetChem 1982;33:19-25.

Fuh CB, Lai M, Tsai HY, Chang CM. Impurity analysis of 1,4-dioxane in nonionic surfactants and cosmetics using headspace solid-phase microextraction coupled with gas chromatography and gas chromatography-mass spectrometry. J Chromatogr A 2005;1071:141-5.

Guo W, Brodowsky H. Determination of the trace 1,4-dioxane. Microchem J 2000;64:173-9.

Black RE, Hurley FJ, Havery DC. Occurrence of 1,4-dioxane in cosmetic raw materials and finished cosmetic products. J AOAC Int 2001;84:666-70.

Zhou W. The determination of 1,4-dioxane in cosmetic products by gas chromatography with tandem mass spectrometry. J Chromatogr A 2019;1607:460400.

TaharaM, ObamaT, IkarashiY. Development of analytical method for determination of 1,4-dioxane in cleansing products. Int J CosmetSci 2013;35:575-80.

Xiyan X, Liu S, Smith K, Wang Y,Hu H. Light-driven breakdown of 1,4-dioxane for potable reuse: A review. ChemEngJ 2019;373:508-18.

Pollitt KJ, Kim J, Peccia J, Elimelech M, Zhang Y, CharkoftakiG, et al. 1,4-dioxane as an emerging water contaminant: State of the science and evaluation of research needs. Sci Total Environ 2019;690:853-66.

US Environmental Protection Agency. 1,4-Dioxane (1,4-Diethyleneoxide). Hazard Summary-Created; 1992.Available from: [Last accessed on2020 Jan].

National Cancer Institute.Bioassay of 1,4-Dioxane for Possible Carcinogenicity. CAS No. 123-91-1. NCI Carcinogenesis Technical Report Series No. 80. NCI-CG-TR80. Bethesda: National Institutes of Health; 1978.

Matheson L, Russell G, MacArthur B,Sheats WB. 1,4-Dioxane-A Current Topic for Household Detergent and Personal Care Formulators 100th AOCS Annual Meeting. Oral Presentation. Available from:

ICH and Q2B.Harmonized Tripartite Guideline, Validation of Analytical Procedure: Methodology, IFPMA, in Proceedings of the International Conference on Harmonization; 1996.

Pappa HN. Validation of compendialprocedures.USP Pharmacopeial Forum 2019;42:8046-52.

Rao KL, Aboul-Enein HY. Elemental impurities determination by ICP-AES/ICP-MS: A review of theory, interpretation of concentration limits, analytical method development challenges and validation criterion for pharmaceutical dosage forms.Curr Pharm Anal 2019;16:1-12.

Rao KL, Reddy KP. Development and validation of a stability-indicating LC method for simultaneous determination of related compounds of guaifenesin, terbutaline sulfate and ambroxolHCl in cough syrup formulation. J Saudi ChemSoc 2014;18:593-600.

Rao KL, Reddy KP. Stability-Indicating method for simultaneous determination of polar and non-polar related compounds of zidovudinein drug substance and drug product tablet form. Int J Res PharmSci 2015;6:5-14.

Dongala T, Katakam LN,PalakurthiAK, Katari NK. RP-HPLC stability indicating method development and validation of pseudoephedrine sulfate and related organic impurities in tablet dosage forms, robustness by QbDapproach. AnalChemLett 2019;9:697-710.

Pathan M, Kshirsagar A. Development of validated stability indicating method by RP-HPLC for simultaneous estimation of meropenemand vaborbactamin bulk and pharmaceutical formulation. Int J PharmPharmSci 2019;11:102-8.

Jamal MK, GazyAA. Development and validation of analytical spectrophotometric and RP-HPLC methods for the simultaneous estimation of hydroquinone, hydrocortisone and tretinointernary mixture in topical formulation. Int J PharmPharmSci2019;11:10-6.

Rao KL. Split-half tablets: A complete review for analytical testing. Asian J Pharm Clin Res 2019;12:27-38.

Rao KL, Rao KP. Development and validation of a stability-indicating LC method for determination of bexarotene in softgel dosage formulation.Chromatographia 2017;80:1211-24.

Rao KL, Reddy KP. Stability-indicating liquid chromatographic method for the simultaneous determination of ascorbic acid, citric acid, butylatedhydroxyanisole, simvastatin and related compounds in pharmaceutical solid dosage form. Int J Anal Pharm Biomed Sci2014;3:1-10.

Rao KL, Reddy KP. Simultaneous estimation of fluticasone propionate, azelastine hydrochloride, phenylethyl alcohol and benzalkonium chloride by RP-HPLC method in nasal spray preparations. Int J Res PharmSci2010;1:473-80.



How to Cite

RAO KATAKAM, L. N., and T. DONGALA. “SELECTIVE TRACE LEVEL DETERMINATION OF 1,4-DIOXANE CONTENT IN SODIUM LAURETH SULFATE RAW MATERIAL BY GAS CHROMATOGRAPHIC-FLAME IONIZATION DETECTION METHOD”. Asian Journal of Pharmaceutical and Clinical Research, vol. 13, no. 6, June 2020, pp. 116-20, doi:10.22159/ajpcr.2020.v13i6.37435.



Original Article(s)