Abstract

An analytical method to measure solubilized orthophosphate ions (HPO42− and PO43− ) from the water-insoluble food additives calcium phosphate dibasic (DCP) and calcium phosphate tribasic (TCP) in processed foods was optimized by comparing ion chromatography (IC) coupled with DS6 conductivity detector (Cond.) and high-performance liquid chromatography (HPLC) with Evaporative light scattering detector (ELSD) methods. The ion-pairing HPLC method could analyze calcium and phosphate ions successively. However, this method exhibited low reproducibility after approximately 48 hours of measurements. The IC method was established as an effective method of measuring orthophosphate ions with high reproducibility using distilled water and KOH solution as the mobile phase with a Dionex column. Matrix-based limit of detections (LOD) and limit of quantifications (LOQ) for snacks and cereals were estimated in the range of 0.01–0.91 µg/mL and 0.21–2.74 µg/mL, respectively. In inter-day and intra-day tests, the calculated precision (%RSD) and accuracy (recovery %) ranged from 0.5% to 6.6% and 82% to 117%, respectively, in both food samples. The levels of DCP or TCP could be analyzed in various positive food samples, and the developed IC method demonstrated good applicability in the analysis of DCP and TCP in collected processed foods.

Highlights

  • Calcium phosphate dibasic (calcium hydrogen phosphate or dicalcium phosphate (DCP)) and calcium phosphate tribasic (tricalcium phosphate (TCP)) are the calcium salt forms of phosphate, which are mainly used as acidity regulators to change or maintain pH in various foods with the EU number of E341(ii) and E341(iii), respectively

  • A peak of orthophosphate from DCP, TCP, and phosphoric acid could be separated from the peak of pyrophosphate (P2 O7 4− ) at 1,000 μg/mL

  • Under all three high-performance liquid chromatography (HPLC) conditions, in which pyrophosphate was eluted as the first peak followed by the peak of orthophosphate, sodium, and calcium

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Summary

Introduction

Calcium phosphate dibasic (calcium hydrogen phosphate or dicalcium phosphate (DCP)) and calcium phosphate tribasic (tricalcium phosphate (TCP)) are the calcium salt forms of phosphate, which are mainly used as acidity regulators to change or maintain pH in various foods with the EU number of E341(ii) and E341(iii), respectively. A survey of the products listed in Korean domestic markets confirmed that they are mainly used for snacks and cereal products They are colorless and tasteless white crystals, which have molecular formulas of CaHPO (a)4 ·2H2 O and Ca3 (PO4 ) with molecular weights of 136.06–172.09 g/mol and 310.18 g/mol, respectively. These phosphate food additives are insoluble in water and ethanol but soluble in dilute hydrochloric acid and nitric acid, resulting in the formation of orthophosphate anions (HPO4 2− and PO4 3− ) [2]. When left in water for an extended time, DCP is converted to the dihydrate form [3]

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