A simultaneous determination method of saccharin (SA), sorbic acid (SOA), benzoic acid (BA),
p-hydroxybenzoic acid ethyl (PHBA-Et),
p-hydroxybenzoic acid isopropyl (PHBA-isoPr),
p-hydroxybenzoic acid propyl (PHBA-Pr),
p-hydroxybenzoic acid isobutyl (PHBA-isoBu) and
p-hydroxybenzoic acid butyl (PHBA-Bu) in foods by HPLC was examined. A mixture of acetonitrile-water (1 : 1) was used to extract these additives from foods excluding liquid foods, while acetonitrile was used to extract them from liquid foods. HPLC was performed using a TSKgel ODS80Ts (4.6 mm i.d.×150 mm) column with a mobile phase of 0.01% formic acid solution containing 2 mmol/L-di-
n-butyl (or amyl) ammonium acetate (A) and acetonitrile (B) under the following conditions: A/B=8 : 2 (0-8 min)→6 : 4 (15-32 min). Recoveries of these additives spiked in foods were 78-120%. The determination limits were 10 μg/g. As the identification method, examination by liquid chromatography with electrospray ionization tandem mass spectrometry (LC/ESI-MS/MS) was used. Unknown compounds were identified by detection of product ions from their precursor ions in the negative mode with multiple reaction monitoring,
m/
z 182>106 for SA,
m/
z 121>77 for BA,
m/
z 111> 67 for SOA and
m/
z 165>92 for PHBA-Et. Ratios of intensity of
m/
z 179>137 to
m/
z 179>92 were used for identification of isomers PHBA-isoPr and PHBA-Pr, and the ratios of intensity of
m/
z 193>137 to
m/
z 193>92 were used for isomers PHBA-isoBu and PHBA-Bu, because these isomers have very similar retention times on HPLC.
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