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Fast and Sensitive Liquid Chromatography Method for Simultaneous Determination of Methylisothiazolinone, Salicylic Acid and Parabens in Cosmetic Products

[ Vol. 13 , Issue. 5 ]

Author(s):

Mohamed Hefnawy*, Abdulrahman Al-Majed, Mostafa Mohammed, Ahmed Al-Ghusn, Adnan Al-Musallam, Nawaf Al-Sowidan, Mishal Al-Hamid and Abdullah Al-Homoud   Pages 430 - 438 ( 9 )

Abstract:


Background: Cosmetic products are required to be safe for consumers under customary conditions of use. Preservatives are used in cosmetics at relatively low concentrations to destroy, block, and prevent the action of any harmful organisms by biological and chemical means. The frequency of allergy to human skin for most preservatives has been described. For quality control of cosmetic products, the determination of these preservatives is essential.

Methods: A simple, rapid and sensitive high-performance liquid chromatography (HPLC) method was developed and validated for the simultaneous determination of preservatives; methylisothiazolinone (MI), salicylic acid (SA), methylparaben (MP), ethylparaben (EP) and propylparaben (PP) in selected cosmetic products. Each compound, together with caffeine (CA) (internal standard) was extracted from the cosmetic matrices with 50% methanol using an ultrasonicator. Chromatography resolution of the preservatives was performed on a Chromolith Speed Rod monolithic silica column (100 mm x 4.6 mm i.d.) with acetonitrile, and 10 mM phosphate buffer (pH 3.0) as the mobile phase under gradient elution conditions. The detection of all compounds was monitored with diode array detection and conducted at ambient temperature.

Results: All preservatives were baseline separated at short run-time (< 8.0 min). The proposed method was validated over the range of 0.3–75 µg mL-1 for MI and 0.1–50 µg mL-1 for SA, MP, EP, PP, respectively, and no correlation coefficients lower than 0.999. The recoveries at the concentrations studied ranged from 95.6% to 103.9% with RSDs less than 3.8%. The proposed method was validated in compliance with ICH guidelines, in terms of accuracy, precision, limits of detection and quantitation and other aspects of analytical validation.

Conclusion: The proposed method is a powerful alternative approach for identifying and determining of the studied preservatives in commercial cosmetic samples. The limits of detection (LODs) and quantitation (LOQs) at the nanogram level were far below the established restrictions in the Saudi Food and Drug Authority Regulation, demonstrating the suitability of the proposed method for routine control. Simple sample pretreatment with monolithic HPLC-PDA developed method produced a selective and accurate analysis without an LC-MS/MS instrument.

Keywords:

Cosmetic, HPLC-PDA, monolithic column, preservative, quantitative analysis, methylisothiazolinone.

Affiliation:

Department of Pharmaceutical Chemistry, College of Pharmacy, King Saud University, Riyadh 11451, Department of Pharmaceutical Chemistry, College of Pharmacy, King Saud University, Riyadh 11451, Department of Pharmaceutical Chemistry, College of Pharmacy, King Saud University, Riyadh 11451, Department of Cosmetic Products Analysis, Saudi Food and Drug Authority (3292), North Ring Road – Al Nafal Unit (1), Riyadh 13312 - 6288, Department of Cosmetic Products Analysis, Saudi Food and Drug Authority (3292), North Ring Road – Al Nafal Unit (1), Riyadh 13312 - 6288, Department of Cosmetic Products Analysis, Saudi Food and Drug Authority (3292), North Ring Road – Al Nafal Unit (1), Riyadh 13312 - 6288, Department of Cosmetic Products Analysis, Saudi Food and Drug Authority (3292), North Ring Road – Al Nafal Unit (1), Riyadh 13312 - 6288, Department of Cosmetic Products Analysis, Saudi Food and Drug Authority (3292), North Ring Road – Al Nafal Unit (1), Riyadh 13312 - 6288

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