Abstract
A method was developed for the separation and determination of benzoic acid in orange juice by high performance liquid chromatography-ultraviolet detection (HPLC-UV) and liquid chromatography-isotope dilution mass spectrometry (LC-IDMS). National Institute of Metrology (NIM) of China participated the international comparison activity organized by Asia Pacific Metrology Programme (APMP) and got good results using this method. The effects of several important factors, such as the chromatographic conditions and sample preparation conditions, were investigated to acquire optimum conditions. A method of uncertainty determination was also developed which can be used in similar measurements of uncertainty. The limit of detection (LOD, S/N > 3) of HPLC-UV method was 0.75 mg/kg, and the recovery of benzoic acid in orange juice at the spiked level 100 mg/kg was 99.4%. The LOD of LC-IDMS method was 0.05 mg/kg, and the recovery of benzoic acid at the same spiked level was 99.6%. The final determination result of benzoic acid in the orange juice sample by both methods was (102.0 +/- 2.1) mg/kg (coverage factor kappa = 2). The two methods are both simple, accurate, reliable and reproducible. The LC-IDMS method is more suitable for the determination of benzoic acid at low concentrations due to its high sensitivity.
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