Validation of an Ion Chromatographic Method for Determination of Anions in Tea Infusions
Iulian Minca, Irina Bajenaru, Cornelia Guran, Ana Maria Joșceanu, Raluca Isopescu
Abstract
Iulian Minca, Irina Bajenaru, Cornelia Guran, Ana Maria Joșceanu, Raluca Isopescu
Abstract
The study is focused on the validation of a simple, rapid, and accurate analysis method for the simultaneous determination of F - , Cl - , Br - , NO 2 - , NO 3 - , SO 4 2- and PO 4 3- ions in white, green, black and Pu-erh tea infusions by ion chromatography with conductometric detection. The high levels of organic components were separated using dedicated filter cartridges. Separation was carried out on an anion-exchange column at 30 o C by isocratic elution with an 4.5 mM Na 2 CO 3 + 1.4 mM NaHCO 3 aqueous eluent. The method proved to be selective, and calibration curves are linear for 0.02 – 10 mg L -1 F - , 0.1 - 50 mg L -1 for Cl - , NO 2 - , Br - , NO 3 - , SO 4 2- , and 0.2 – 100 mg L -1 PO 4 3- , characterized by slopes of 0.07 - 0.32, with standard deviations, s b , of 0.03 – 0.14, intercepts of 0.00 – 0.01 mg L -1 , standard deviations of intercepts, s a , of 0.62 - 2.50 mg L -1 , and correlation coefficients of 0.999 for each ion of interest. The calculated limits of detection and quantification for independent fortified samples were in the 0.004 - 0.019 mg L -1 and 0.014 – 0.064 mg L -1 range, respectively. Repeatability and intermediate precision tests gave RDS% between 0.04 % and 0.37 %, values, significantly lower than the imposed limit. The recovery of various anions in spiked tea samples varied in the 95.2 - 114 % range. The method was successfully applied for the anionic content of 60 tea types available in Romanian shops.
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The study is focused on the validation of a simple, rapid, and accurate analysis method for the simultaneous determination of F - , Cl - , Br - , NO 2 - , NO 3 - , SO 4 2- and PO 4 3- ions in white, green, black and Pu-erh tea infusions by ion chromatography with conductometric detection. The high levels of organic components were separated using dedicated filter cartridges. Separation was carried out on an anion-exchange column at 30 o C by isocratic elution with an 4.5 mM Na 2 CO 3 + 1.4 mM NaHCO 3 aqueous eluent. The method proved to be selective, and calibration curves are linear for 0.02 – 10 mg L -1 F - , 0.1 - 50 mg L -1 for Cl - , NO 2 - , Br - , NO 3 - , SO 4 2- , and 0.2 – 100 mg L -1 PO 4 3- , characterized by slopes of 0.07 - 0.32, with standard deviations, s b , of 0.03 – 0.14, intercepts of 0.00 – 0.01 mg L -1 , standard deviations of intercepts, s a , of 0.62 - 2.50 mg L -1 , and correlation coefficients of 0.999 for each ion of interest. The calculated limits of detection and quantification for independent fortified samples were in the 0.004 - 0.019 mg L -1 and 0.014 – 0.064 mg L -1 range, respectively. Repeatability and intermediate precision tests gave RDS% between 0.04 % and 0.37 %, values, significantly lower than the imposed limit. The recovery of various anions in spiked tea samples varied in the 95.2 - 114 % range. The method was successfully applied for the anionic content of 60 tea types available in Romanian shops.
Key concepts: Chemistry, Detection limit, Ion chromatography, Chromatography, Repeatability, Calibration curve, Analytical Chemistry (journal), Elution