Determination of Total Iodine in Infant Formula and Nutritional Products by Inductively Coupled Plasma/Mass Spectrometry: Single-Laboratory Validation

2012 ◽  
Vol 95 (1) ◽  
pp. 169-176 ◽  
Author(s):  
Lawrence H Pacquette ◽  
Alan M Levenson ◽  
Joseph J Thompson

Abstract A single-laboratory validation by inductively coupled plasma-mass spectrometry was developed for the determination total iodine (m/z 127) in infant formula and adult nutritional products. All samples were digested in nitric acid using a closed vessel microwave oven system; Te (m/z 130) was used as an internal standard. To prevent loss of iodine, ammonium hydroxide solution was added to the samples immediately after digestion. The method quantitation limit for total iodine was 0.3 ng/mL, but a practical LOQ was used at 1.0 ng/mL, a concentration at which there was a negligible bias due to nonlinearity. The total iodine concentrations (112–1900 ng/g) in 14 out of 15 nutritional products were within specification limits. Within-day and day-to-day (6 independent days) precision values were <10% RSD. The observed precision for the overall mean (18 independent days) of a control sample was approximately 4% RSD. In two National Institute of Standards and Technology standard reference materials, total iodine results were within certified limits. Sample spike recoveries for all 15 nutritional products were 92–105%. The data show that a conventional microwave oven digestion procedure can be used to prepare samples for iodine determination. Therefore, this technique is very compatible with other methods being proposed as modern official methods for the analysis of minerals in nutritional products.

2016 ◽  
Vol 99 (3) ◽  
pp. 766-775 ◽  
Author(s):  
Lawrence H Pacquette ◽  
Anil Anumula

Abstract A method was developed for the determination of As, Cd, Hg, and Pb in raw ingredients, nutritional products, and infant formula using inductively coupled plasma mass spectrometry (ICP-MS). Three raw ingredients (acid casein, maltodextrin, skim milk powder) and three standard reference materials [NIST 1548a (Typical Diet), NIST 1577c (Bovine Liver), NIST SRM 1568b (Rice Flour)] obtained from the National Institute of Standards and Technology were analyzed by two analysts using two ICP-MS instruments in different laboratories. NIST SRM 1568b was used as the control sample. All protocol validation parameters (intermediate precision, accuracy, linearity, quantitation limit, specificity, and robustness) were met. The overall precision (n = 8) for analyte concentrations (2.5–300 ng/g) ranged from 2 to 14% RSD. Spike recoveries ranged from 88 to109% for spike levels between 25 and 200%. The overall average concentration of As, Cd, Hg, and Pb measured in all three NIST SRMs were within the certified value ranges. Good linearity (correlation coefficient (r) = 0.9995 or better) was obtained for all analytes. Control chart results for 8 independent days showed that the method is robust (precision values of 10% and all points within ±3 σ were obtained). Excellent specificity was also demonstrated when the analytes were measured in the presence of high concentrations of the other concomitants.


1993 ◽  
Vol 76 (6) ◽  
pp. 1378-1384 ◽  
Author(s):  
Joseph J Thompson

Abstract A simple method was developed for the accurate and precise determination of low- and sub-ppb (ng/g) concentrations of lead in infant formula by isotope dilution inductively coupled plasma mass spectrometry using ultrasonic nebulization. After addition of a known amount of 207Pb, samples were microwave digested and the ratio 207Pb/208Pb was measured in the digests. Agreement with certified values for lead in milk powder standard reference materials was good, and isotope dilution analysis using 206Pb yielded identical results for the standard reference materials. Lead concentrations determined for several infant nutritional products were verified by an independent method. Typically, relative standard deviations of <4% were obtained with this method for lead concentrations above 2 ppb. The recovery of 2 ng of lead from an aqueous standard carried through the microwave digestion was 104 ± 4%. Infant formula (containing 0.6 ppb lead) to which 0.4 ng of natural-abundance lead had been added, to simulate a formula containing 0.9 ppb lead, was analyzed by isotope dilution, and the result was 96 ± 18% of the theoretical value. Thus, differences of 0.3 ppb lead could be clearly distinguished, and the detection limit was estimated to be 0.1 ng lead per gram of infant formula. The keys to accuracy for this method are minimizing contamination and accurately determining the concentration of lead in the isotopically enriched standard.


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