Website: https://vjfc.nifc.gov.vn/
Website: https://vjfc.nifc.gov.vn/
A high-performance liquid chromatography coupled with photodiode array detection (HPLC-PDA) method was developed and validated for the simultaneous determination of nine preservatives, including benzoic acid (BA), sorbic acid (SA), methylparaben (MP), ethylparaben (EP), propylparaben (PP), isopropylparaben (iPP), phenylparaben (PheP), butylparaben (BP), and isobutylparaben (iBP), in dietary supplements. Samples were extracted by ultrasound-assisted extraction with 80% methanol for 10 min and purified using Carrez reagents. Chromatographic separation was performed on a SilicaChrom® C18 column using methanol and 20 mM ammonium acetate buffer (pH 4.3) under gradient elution, with detection at 230 nm for BA and 254 nm for the remaining analytes, and an injection volume of 20 μL. The method was validated according to the International Council for Harmonisation of Technical Requirements for Pharmaceuticals for Human Use (ICH Q2(R2)) guideline and demonstrated satisfactory specificity, linearity, sensitivity, accuracy, precision, and robustness. Working ranges were 0.5 - 20 mg/L for most analytes, with limit of detection (LOD) and limit of quantitation (LOQ) of 0.02 - 1.34 mg/kg and 0.07 - 4.07 mg/kg, respectively. Recoveries ranged from 90.8% to 109.2%, and repeatability and intermediate precision showed relative standard deviations below 2%. The method was applied to the analysis of 41 commercial health supplement samples. The estimated dietary exposure levels of the detected preservatives were below the corresponding acceptable daily intake (ADI) values established by JECFA. However, when compared with the current Vietnamese regulation QCVN 4-12:2010/BYT, the estimated exposure exceeded the corresponding ADI for some products, particularly among children.
HPLC, dietary supplements, preservatives, parabens, dietary exposure assessment.
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