New (31)P NMR internal reference standard - hexamethylphosphoroamide (HMPA) was applied for determination of added polyphosphates and their ionic forms in raw pork meat and meat products. Phosphate species were determined after extraction with a boric acid buffer (pH=9) and EDTA solution, using internal standard (HMPA) procedure. Hexamethylphosophoroamide was also used as the NMR reference standard. Linear correlations between phosphates and polyphosphate concentrations and (31)P NMR signal areas were found in the range 81-5236 mg P/dm(3), presenting 95-99% recovery and variation coefficient (CV) ≤ 5%. Studied HMPA procedure revealed shorter analysis time and the same recovery (>95%) and precision (CV=1.3-2.7%) in comparison to MDPA method. Results of phosphate determination by both (31)P NMR methods were tested against the molybdenumvanadate yellow spectrophotometric method (standard PN-ISO 13730, 1999) using standard reference material (certified phosphate solution).
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http://dx.doi.org/10.1016/j.talanta.2010.12.046 | DOI Listing |
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