Total Iodine in Infant Formula and Nutritional Products by Inductively Coupled Plasma/Mass Spectrometry: First Action 2012.14

2013 ◽  
Vol 96 (4) ◽  
pp. 798-801 ◽  
Author(s):  
Lawrence H Pacquette ◽  
Alan M Levenson ◽  
Joseph J Thompson ◽  
Dawn Dowell
Keyword(s):  
Infant Formula ◽  
Inductively Coupled Plasma ◽  
Internal Standard ◽  
Total Iodine ◽  
Method Performance ◽  
Inductively Coupled ◽  
Expert Review ◽  
Performance Requirements ◽  
Expert Review Panel ◽  
Plasma Mass Spectrometry

Abstract After an assessment of data generated from a single-laboratory validation study published in the Journal of AOAC INTERNATIONAL 95, 169–176 (2012), a method for determining the total level of iodine in infant formula and nutritional products was presented for consideration for adoption by AOAC during the AOAC Annual Meeting held September 30–October 3, 2012 in Las Vegas, NV. An Expert Review Panel on Infant Formula and Adult Nutritionals concluded that the method met the established standard method performance requirements, and approved the method as AOAC Official First Action. The method involves digestion of the sample with nitric acid in a closed vessel microwave oven, followed by determination by inductively coupled plasma/MS using tellurium as the internal standard. The method LOQ for total iodine was 1.5 μg/100 g, but a practical LOQ was used at 5 μg/100 g total iodine. The analytical range of the method was 5–100 μg/100 g total iodine. The recoveries from 15 spiked nutritional products ranged from 90 to 105%.

scholarly journals Chloride in Milk, Milk Powder, Whey Powder, Infant Formula, and Adult Nutritionals Potentiometric Titration: Collaborative Study, Final Action 2016.03

2019 ◽  
Vol 102 (2) ◽  
pp. 564-569
Author(s):  
Greg Jaudzems ◽  
Fengxia Zhang ◽  
Wu Bolong ◽  
Lei Bao ◽  
Jing Xiao
Keyword(s):  
Infant Formula ◽  
Collaborative Study ◽  
Milk Powder ◽  
Method Performance ◽  
Expert Review ◽  
Performance Requirements ◽  
Expert Review Panel ◽  
Repeatability And Reproducibility ◽  
Set Up ◽  
Single Laboratory

Abstract Background: In September 2015, both AOAC Official Methods 2015.07and 2015.08 single-laboratory validations (SLVs) were reviewed against Standard Method Performance Requirements® (SMPR) 2014.015by the AOAC Stakeholder Panel for Infant Formula andAdult Nutritional (SPIFAN) Expert Review Panel (ERP). Looking at the similarity and uniqueness of the two methods, the authors agreed, as advised by the ERP, to work together to merge the two methods intoone. This combined method was assigned Method 2016.03. Objective: In order to determine the repeatability and reproducibility of the AOAC First Action 2016.03 method, a collaborative study was organized. The study was divided in two parts: (Part 1) method set up and qualification of participants and (Part 2) collaborative study participation. During Part 1, each laboratory was asked to analyze two practice samples. The laboratories that provided results within a range of expected levels were qualified for Part 2, during which they analyzed 25 samples in blind duplicates. Results: The results were compared with SMPR 2014.015 established for chloride. The precision results (repeatability and reproducibility) were within therequirements stated in the SMPR. In general, the precision results (repeatability and reproducibility)were well within the limits stated in the SMPR. Repeatability ranged from 0.4 to 1.9%, in accordance with data obtained during SLV, with reported RSD of repeatability from 0.03 to 1.6%. Meanwhile, reproducibility ranged from 0.6 to 4.0%. Finally, the Horwitz ratio values were all below 1, from 0.2 to 0.9%. Conclusions: The ERP determined that the data presented met the SMPR and accordingly recommended the method to be granted Final Actionstatus. In January 2018, the Official Methods Boardapproved the method as Final Action.

Application of Inductively Coupled Plasma/Mass Spectrometry for the Measurement of Chromium, Selenium, and Molybdenum in Infant Formula and Adult Nutritional Products: First Action 2011.19

2012 ◽  
Vol 95 (3) ◽  
pp. 588-598 ◽  
Author(s):  
Lawrence H Pacquette ◽  
Andre Szabo ◽  
Joseph J Thompson ◽  
Steve Baugh
Keyword(s):  
Infant Formula ◽  
Inductively Coupled Plasma ◽  
Internal Standard ◽  
Reference Method ◽  
Standard Reference Materials ◽  
Internal Standards ◽  
Inductively Coupled ◽  
Technology Standard ◽  
Plasma Mass Spectrometry

Abstract An inductively coupled plasma/MS method was developed for the simultaneous determination of Cr, Se, and Mo in infant formula and other nutritional products. All samples were digested using a closed vessel microwave oven system, together with Ni and Te internal standards. The practical quantitation limits for Cr, Se, and Mo were 0.4, 0.2, and 0.4 ng/mL, respectively; dilution factors were 250 for powders and 50 for liquids. The Cr, Se, and Mo concentrations in 10 nutritional products were within specification limits; within-day and day-to-day (6 independent days) precision values were <5% RSD. For two control samples, the observed precision was ≤2% RSD over 10 independent days. Cr, Se, and Mo results were within the certified limits in three National Institute of Standards and Technology standard reference materials. The average sample spike recoveries for 10 nutritional products ranged from 93 to 107%. Robustness studies showed a minimal effect from concomitant easily ionized element concentrations. However, the choice of internal standard and matrix-matching carbon content were critical to obtaining accurate Se results. All indications are that this method would be a suitable candidate as a global reference method for the determination of these trace elements in infant formula, adult nutritionals, and other nutritional products.

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
Keyword(s):  
Mass Spectrometry ◽  
Infant Formula ◽  
Inductively Coupled Plasma ◽  
Control Sample ◽  
Microwave Oven ◽  
Standard Reference Materials ◽  
Total Iodine ◽  
Inductively Coupled ◽  
Plasma Mass Spectrometry ◽  
Single Laboratory

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.

scholarly journals Total Amino Acids by UHPLC–UV in Infant Formulas and Adult Nutritionals, First Action 2018.06

2019 ◽  
Vol 102 (5) ◽  
pp. 1574-1588 ◽  
Author(s):  
Greg Jaudzems ◽  
Joseph Guthrie ◽  
Sabine Lahrichi ◽  
Christophe Fuerer
Keyword(s):  
Amino Acids ◽  
Infant Formula ◽  
Amino Acid Content ◽  
Method Performance ◽  
Expert Review ◽  
Performance Requirements ◽  
Expert Review Panel ◽  
Single Laboratory ◽  
Total Amino Acids

Abstract Background: An acid hydrolysis ultrahigh-performance LC–UV method was evaluated for the determination of total amino acids in infant formula and adult/pediatric nutritional formula. Objective: It was assessed for compliance against AOAC INTERNATIONAL Standard Method Performance Requirements (SMPR®) established by the Stakeholder Panel for Infant Formula and Adult Nutritionals (SPIFAN). Methods: A single-laboratory validation (SLV) study was conducted as a first step in the process to validate the method. In this SLV, 17 SPIFAN matrices representing a range of infant formula and adult nutritional products were evaluated for their amino acid content. Results: The analytical range was found to be within the needs for all products; some may require a dilution. Evaluation of trueness performed on Standard Reference Material 1849a (Infant/Adult Nutritional Formula) showed all compounds met the SMPR theoretical value, with exceptions for threonine and tyrosine. These may have a bias for the National Institute of Standards and Technology (NIST) data, depending on hydrolysis used in the determination of the NIST certificate of analysis. Conclusions: Based on the results of this SLV, this method met the SMPR and was approved as a First Action method by the AOAC Expert Review Panel on Nutrient Methods on August 28, 2018.

Total Folate in Infant Formula and Adult Nutritionals by Trienzyme Extraction and LC-MS/MS Quantitation: A Multilaboratory Testing Study, Final Action 2011.06

2018 ◽  
Vol 101 (6) ◽  
pp. 1881-1894 ◽  
Author(s):  
Sneh D Bhandari ◽  
Ming Gao ◽  
John Szpylka ◽  
N Collopy ◽  
H Chen ◽  
...  
Keyword(s):  
Infant Formula ◽  
Collaborative Study ◽  
Reference Method ◽  
Official Method ◽  
Method Performance ◽  
Expert Review ◽  
Performance Requirements ◽  
Relative Standard ◽  
Expert Review Panel ◽  
Repeatability And Reproducibility

Abstract Background: The need for an updated reference method for folate was identified as a priority by the AOAC’s Stakeholder Panel on Infant Formula and Adult Nutritionals (SPIFAN) in 2011. An Expert Review Panel (ERP) found AOAC Official MethodSM 2011.06 suitable for the purpose and approved it as a First Action Official Method. Objective: To determine the repeatability and reproducibility of Method 2011.06: Total Folate in Infant Formula and Adult Nutritionals by Trienzyme Extraction and LC-MS/MS Quantitation. Methods: A multilaboratory collaborative study was conducted. Eleven laboratories located in five countries participated and completed analysis of all multilaboratory testing (MLT) samples. The study was divided into two parts. In the first part, the laboratories analyzed two practice samples (blindly coded) using the updated folate Method 2011.06. The laboratories providing results within the expected range qualified for part two, in which they analyzed 11 MLT samples in blind duplicates. Results: The results were compared with the Standard Method Performance Requirements (SMPR 2011.006) established for folate. The precision results met the requirements stated in the SMPR for all of the samples. Repeatability and reproducibility relative standard deviations ranged from 3.5 to 6.6 and from 9.0 to 15.7%, respectively. Horwitz ratio values for all of the samples were well below 2 (0.61–1.06). Conclusions: The ERP determined that the method performance met the SMPR requirements in September 2017 after reviewing the presented MLT data. Highlights: The ERP recommended the method for Final Action status.

Determination of Chromium, Selenium, and Molybdenum in Infant Formula and Adult Nutritional Products by Inductively Coupled Plasma/Mass Spectrometry: Collaborative Study, Final Action 2011.19

2015 ◽  
Vol 98 (6) ◽  
pp. 1702-1710 ◽  
Author(s):  
Lawrence H Pacquette ◽  
Joseph J Thompson ◽  
M Farrow ◽  
M Feller ◽  
Y Fenpeng ◽  
...  
Keyword(s):  
Infant Formula ◽  
Inductively Coupled Plasma ◽  
Microwave Digestion ◽  
Collaborative Study ◽  
Simultaneous Detection ◽  
Internal Standard ◽  
Reaction Cell ◽  
Method Performance ◽  
Inductively Coupled ◽  
Icp Ms

Abstract AOAC First Action Method 2011.19: Chromium, Selenium, and Molybdenum in Infant Formula and Adult Nutritional Products, was collaboratively studied. This method uses microwave digestion of samples with nitric acid, hydrogen peroxide, and internal standard followed by simultaneous detection of the elements by an inductively coupled plasma (ICP)/MS instrument equipped with a collision/ reaction cell. During this collaborative study, nine laboratories from four different countries, using seven different models of ICP/MS instruments, analyzed blind duplicates of seven infant, pediatric, and adult nutritional formulas. One laboratory's set of data was rejected in its entirety. The method demonstrated acceptable repeatability and reproducibility and met the AOAC Stakeholder Panel on Infant Formula and Adult Nutritionals (SPIFAN) Standard Method Performance Requirements (SMPRs®) for almost all of the matrixes analyzed. The Cr, Mo, and Se SPIFAN requirement for repeatability was ≤5% RSD. The SMPR called for a reproducibility of ≤15% RSD for products with ultratrace element concentrations above the targeted LOQ of 20 μg/kg Cr/Mo and 10 μg/kg Se (as ready-to-feed). During this collaborative study, RSDr ranged from 1.0 to 7.0% and RSDR ranged from 2.5 to 13.4% across all three ultratrace elements.

Simultaneous Determination of Vitamins D2 and D3 by LC-MS/MS in Infant Formula and Adult Nutritionals: First Action 2011.13

2012 ◽  
Vol 95 (3) ◽  
pp. 583-587 ◽  
Author(s):  
Donald L Gilliland ◽  
Charles K Black ◽  
James E Denison ◽  
Charles T Seipelt ◽  
Dawn Dowell
Keyword(s):  
Simultaneous Determination ◽  
Infant Formula ◽  
Practical Method ◽  
Intermediate Precision ◽  
Method Performance ◽  
Expert Review ◽  
Performance Requirements ◽  
Expert Review Panel ◽  
Working Standards

Abstract During the “Standards Development and International Harmonization: AOAC INTERNATIONAL Mid-Year Meeting” held on June 29, 2011, an Expert Review Panel (ERP) on behalf of AOAC INTERNATIONAL adopted the method “Simultaneous Determination of Vitamins D2 and D3 by LC-MS/MS in Infant Formula and Adult Nutritionals” as an AOAC Official First Action method. Vitamins D2 and D3 are extracted from the sample using pentane–ether; the extract is collected and dried under nitrogen. Vitamin D is separated from interfering compounds using UPLC, and quantitated using tandem mass spectrometry (MS/MS). Preliminary data showed the intermediate precision ranged from 3.34–8.05% and an accuracy range of 98.5–111% over the samples tested for vitamin D3. For vitamin D2, the intermediate precision ranged from 2.37–5.45% and accuracy ranged from 96.4–104% over the four matrixes evaluated. The analytical range for the method is bounded by the concentrations of the working standards, 21–270 ng/mL, and is equivalent to 0.168–2.16 mcg/100 g in ready-to-feed product. The practical method quantitation limit is 0.168 mcg/100 g product with method detection limit of 60 ng/100 g product. The ERP reviewed the data and determined that the performance characteristics of the method met the standard method performance requirements, and therefore the method was granted First Action status.

Sign in / Sign up

Export Citation Format

Share Document