engleski

Determination of corticosteroids using liquid chromatography/ time-of-flight mass spectrometry

Undeclared corticosteroids in products intended for frequent use might cause serious side- effects. In order to prevent this or find the cause, it was essential to develope a method for quick detection and quantification. This work investigated the applicability of reversed-phase liquid chromatography coupled to time-of-flight mass spectrometry (LC-TOF-MS) for qualitative and quantitative determination of corticosteroids in different cosmetic products and dietary supplements. Nine corticosteroids were used: prednisone, prednisolone, hydrocortisone, dexamethasone, hydrocortisone acetate, triamcinolone acetonid, clobetasole propionate, betamethasone dipropionate and alclomethasone dipropionate. Separation was achived under 15 min on an Inertsil ODS-4 C18 column using gradient eluation with 5 mmol L-1 ammonium acetate in water and acetonitrile as mobile phases at a flow rate of 0, 3 mL min-1. The detection was performed with a TOF mass spectrometer in positive polarity equipped with an electrospray interface. Identification was based on accurate mass measurement of protonated ion [M+H]+ and LC retention time of the analyte compared to the standard. The method was validated in terms of specificity, precision, accuracy, detection and quantification limits, linearity and recovery. The validation parametars met all acceptance criteria. An LC-TOF method was developed and validated for the rapid and simultaneous determination of nine corticosteroids. The proposed method can be used for testing different product such as dietary supplements and cosmetic products (creams and ointments). Regular and consistent monitoring of the use of corticosteroids is needed. However, additional efforts are needed to improve the extraction of analytes from different matrices.

Cosmetic products ; dietary supplements ; LC-TOF-MS ; quality control

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