Palmerston North, New Zealand
Palmerston North, New Zealand

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Mahmoodani F.,University of Auckland | Perera C.O.,University of Auckland | Fedrizzi B.,University of Auckland | Abernethy G.,Fonterra Cooperative Group Ltd | Chen H.,Fonterra Cooperative Group Ltd
Food Chemistry | Year: 2017

In any food fortification program, the stability of added micronutrients is an important factor. Cholecalciferol or vitamin D3 is known to isomerise under various conditions, thereby making its analysis challenging. In the current study, the effects of different parameters, such as temperature, iodine, acidic conditions, and oxidation, on the isomerisation of vitamin D3 were studied using HPLC-DAD and UHPLC-MS/MS. Vitamin D3 thermally and reversibly transforms to pre-vitamin D3 type isomers. In the presence of iodine, cis/trans isomerisation of both cholecalciferol and pre-vitamin D3 takes place to form trans-vitamin D3 and tachysterol, respectively. Another isomer, isotachysterol, was formed under acidic conditions. The different rates of reaction of these products with a dienophile through the Diels-Alder reaction confirmed the formation of vitamin D3 isomerisation products. The derivatization enhanced the ionisation efficiency of vitamin D3 and its isomers in UHPLC-MS/MS and improved the separation and fragmentation enabling sensitive detection. © 2016 Elsevier Ltd


Woollard D.C.,New Hill | Bensch A.,New Zealand Laboratory Services | Indyk H.,Fonterra Cooperative Group Ltd | McMahon A.,Wyeth Nutrition
Food Chemistry | Year: 2016

An HPLC method is described using normal phase conditions with an unbonded silica column to determine concentrations of supplementary vitamin A and vitamin E esters and β-carotene in infant formulae. The method utilises selective dual-channel fluoresence for vitamins A and E and visible absorbance for β-carotene. An attribute of the method is the use of retinol propionate, α-tocopheryl propionate and all-E-β-apo-8′-carotenoic acid ethyl ester internal standards to compensate for analytical variations associated with these labile vitamins. Extraction is performed without saponification, with the aid of protease to remove vitamin encaspsulation and facilitate vitamin partition into hydrocarbon solvent. Figures of merit indicate the method is suitable for its intended purpose in the highly regulated infant formula environment, including liquid formulations. The method is extendable to whole milk powders where total vitamin A content data can be calculated by summing the innate long-chain vitamin A esters with the added esters. © 2015 Elsevier Ltd.


PubMed | Fonterra Cooperative Group Ltd, Wyeth Nutrition, New Zealand Laboratory Services and New Hill
Type: Journal Article | Journal: Food chemistry | Year: 2015

An HPLC method is described using normal phase conditions with an unbonded silica column to determine concentrations of supplementary vitamin A and vitamin E esters and -carotene in infant formulae. The method utilises selective dual-channel fluoresence for vitamins A and E and visible absorbance for -carotene. An attribute of the method is the use of retinol propionate, -tocopheryl propionate and all-E--apo-8-carotenoic acid ethyl ester internal standards to compensate for analytical variations associated with these labile vitamins. Extraction is performed without saponification, with the aid of protease to remove vitamin encaspsulation and facilitate vitamin partition into hydrocarbon solvent. Figures of merit indicate the method is suitable for its intended purpose in the highly regulated infant formula environment, including liquid formulations. The method is extendable to whole milk powders where total vitamin A content data can be calculated by summing the innate long-chain vitamin A esters with the added esters.


Gill B.D.,Fonterra Cooperative Group Ltd | Indyk H.E.,Fonterra Cooperative Group Ltd | Blake C.J.,Nestlé | Konings E.J.M.,Nestlé | And 2 more authors.
Journal of AOAC International | Year: 2015

Methods under consideration as part of the AOAC Stakeholder Panel on Infant Formula and Adult Nutritionals process are to be evaluated against a set of Standard Method Performance RequirementsSM (SMPRs) via peer review by an expert review panel (ERP). A validation protocol and a checklist have been developed to assist the ERP to evaluate experimental data and to compare multiple candidate methods for each nutrient. Method performance against validation parameters mandated in the SMPRs as well as additional criteria are to be scored, with the method selected by the ERP proceeding to multilaboratory study prior to Final Action approval. These methods are intended to be used by the infant formula industry for the purposes of dispute resolution.


Woollard D.C.,New Hill | Macfadzean C.,New Zealand Laboratory Services Ltd. | Indyk H.E.,Fonterra Cooperative Group Ltd. | McMahon A.,Wyeth Nutrition | Christiansen S.,Perrigo Nutritionals PBM Products
International Dairy Journal | Year: 2014

A gas chromatography-flame ionisation detection method was developed to establish the content of myo-inositol in milk powders and infant formulations subsequent to formation of the volatile trialkylsilyl derivative. Samples were prepared by acid digestion, thereby releasing inositol from its multiple bound forms. A digestion time of 4h at 114°C was sufficient to hydrolyse potentially interfering carbohydrates and quantitatively recover bound inositol from milk-based products. Single laboratory method validation showed a within-day relative standard deviation (RSDr) of 5.9% and between-day relative standard deviation (RSDiR) of 9.6%. A between-laboratory (n=7) collaborative study yielded an average reproducibility (RSDR) of 12.8%, considered fit-for-purpose as a quality control method for milk-based infant formulations. Soy-based products, containing significant inositol hexaphosphate (IP6, phytic acid), required 32h for release of all inositol. Although current regulations do not specify the inclusion of IP6 in an inositol measurement, the current method allows for its discrimination if present. © 2014 Elsevier Ltd.


Andrewes P.,Fonterra Cooperative Group Ltd | Bendall J.G.,Fonterra Cooperative Group Ltd | Davey G.,Fonterra Cooperative Group Ltd | Shingleton R.,Fonterra Cooperative Group Ltd
International Dairy Journal | Year: 2010

A musty flavour defect in calcium caseinate that was due to tainting by 2,4,6-tribromoanisole (TBA) is described. The concentration of TBA in tainted calcium caseinate was between 2 and 560 μg kg-1; substantially above the sensory threshold (0.02 μg kg-1 in a 10% calcium caseinate solution). The TBA was derived from 2,4,6-tribromophenol (TBP) that had contaminated materials that were used in the calcium caseinate supply chain. TBP is readily converted to TBA by environmental fungi. Potential TBP sources identified in this investigation were timber shipping container floors, and slipsheets constructed from recycled plastics that were used for transporting stacks of calcium caseinate. The TBP sources identified were consistent with trends in the increased industrial use of this chemical in wood products and plastics. © 2010 Elsevier Ltd. All rights reserved.


Andrewes P.,Fonterra Cooperative Group Ltd
Food Chemistry | Year: 2012

Ghee (milkfat from heat clarification) was made using direct cream (DC), cream butter (CB) or pre-stratification (PS) methods and stored at 60 °C, in air, for at least two weeks. Milkfat degradation, particularly oxidation, occurred in all types of ghee, resulting in increases in aldehydes and free fatty acids. However, there was little difference in fat degradation rates in each type of ghee. DC and CB ghee contained volatile Maillard reaction products, whereas PS ghee did not. The concentrations of 3,4-dihydroxy-3-hexen-2,5-dione (DHHD) and 2,3-dihydro-3,5-dihydroxy-6-methyl-4(H)-pyran-4-one (pyranone), Maillard reaction products found in DC and CB ghee, rapidly decreased during storage, associated with increases in acetic acid. This work suggests hydration of both DHHD and pyranone, during storage, could form reactive 1-deoxy-d-erythro-hexo-2,3-diulose (1-deoxyglucosone) that degrades mostly to acetic acid. Thus, the Maillard reaction cascade appears to continue in food, in the absence of proteins and sugars, long after cooking has ceased. © 2012 Elsevier Ltd. All rights reserved.


Woollard D.C.,Cawthron Institute | Indyk H.E.,Fonterra Cooperative Group Ltd.
International Dairy Journal | Year: 2014

A manual method is described for the determination of nitrate and nitrite in milk and milk powders that is intended to provide an alternative to conventional manual methods accomplished by cadmium reduction. Reduction of nitrate is performed in solution utilising vanadium (III) and quantitation achieved by concurrent reaction with Griess reagent. Performance data are acceptable in terms of precision and accuracy, repeatability being about 6% and intermediate precision at 8% for both analytes, providing the limit of detection is not approached. Limit of quantitation is 0.1mgkg-1 for both analytes. © 2013.


PubMed | University of Auckland and Fonterra Cooperative Group Ltd
Type: | Journal: Food chemistry | Year: 2016

In any food fortification program, the stability of added micronutrients is an important factor. Cholecalciferol or vitamin D3 is known to isomerise under various conditions, thereby making its analysis challenging. In the current study, the effects of different parameters, such as temperature, iodine, acidic conditions, and oxidation, on the isomerisation of vitamin D3 were studied using HPLC-DAD and UHPLC-MS/MS. Vitamin D3 thermally and reversibly transforms to pre-vitamin D3 type isomers. In the presence of iodine, cis/trans isomerisation of both cholecalciferol and pre-vitamin D3 takes place to form trans-vitamin D3 and tachysterol, respectively. Another isomer, isotachysterol, was formed under acidic conditions. The different rates of reaction of these products with a dienophile through the Diels-Alder reaction confirmed the formation of vitamin D3 isomerisation products. The derivatization enhanced the ionisation efficiency of vitamin D3 and its isomers in UHPLC-MS/MS and improved the separation and fragmentation enabling sensitive detection.


PubMed | Fonterra Cooperative Group Ltd
Type: Journal Article | Journal: Journal of AOAC International | Year: 2015

Methods under consideration as part of the AOAC Stakeholder Panel on Infant Formula and Adult Nutritionals process are to be evaluated against a set of Standard Method Performance RequirementsSM (SMPRs) via peer review by an expert review panel (ERP). A validation protocol and a checklist have been developed to assist the ERP to evaluate experimental data and to compare multiple candidate methods for each nutrient. Method performance against validation parameters mandated in the SMPRs as well as additional criteria are to be scored, with the method selected by the ERP proceeding to multilaboratory study prior to Final Action approval. These methods are intended to be used by the infant formula industry for the purposes of dispute resolution.

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