Carrageenan analysis. Part 2: Quantification in swine-adapted infant formula

Abstract

An LC-MS/MS method was validated in accordance with 21CFR Part 58 Good Laboratory Practice for Non-clinical Laboratory Studies to measure the concentration of carrageenan in dose formulations used in a 28-day piglet dietary feeding study of swine-adapted infant formulations stabilised with carrageenan. Carrageenan concentrations in the test formulations were 0, 300, 1000 and 2250 mg kg^–1 formula. The method for the measurement of carrageenan was LC-MS/MS coupled with ESI in negative-ion mode for detection. Linearity was established over the range 1.00–7.50 µg ml^–1. Carrageenan dose formulation samples ranging from 0 to 2250 mg kg^–1 of carrageenan were diluted to within the linearity range for measurement.

Keywords:

• carrageenan
• infant formula
• swine-adapted infant formula
• LC-MS/MS
• ESI

Acknowledgements

The authors thank: Abbott Nutrition for development and production of the swine-adapted test formulations; Bjorn A. Thorsrud, Study Director (MPI), and Kimberly S. Roberts (MPI Research) for data verification; Ashley F. Brant (MPI Research), Myra L. Weiner (TOXpertise LLC), Brinda Mahadevan (Abbott Nutrition), and Christopher J. Sewall (FMC) for technical discussions; and Eunice M. Cuirle (FMC), Theresa M. Hedrick (IFC), and Brenda Frantz (MPI Research) for project management and coordination. The authors are identified above. William Blakemore is the owner and principal of Celtic Colloids Inc., a consulting company providing advice on hydrocolloids technology and including leadership on analytical methods development to private companies. Karina Kwok is an Associate Principal Scientist at MPI Research responsible for the development and validation of the method for the measurement of carrageenan in swine-adapted infant formula, and the application of the validated method to the analysis of swine-adapted infant formula samples used in non-clinical studies. Niles Harding was previously a Research Specialist with MPI Research and performed the experiments associated with the development, validation and sample analysis for infant formula. The research work detailed in this paper was carried out for FMC Corporation (FMC) and the International Formula Council (IFC) under cost reimbursable contracts. FMC is a manufacturer of carrageenan and products containing carrageenan. The IFC is an association of manufacturers and markers of formulated nutrition products, e.g. infant formulas and adult nutritionals, whose members are based predominantly in North America. The method development and validation reported in this paper is the professional work product of the authors. FMC and IFC were given the opportunity to review this paper and to offer comments on the content. Those comments did not alter the professional opinions of the authors. The authors have not appeared in any legal proceedings related to the findings reported in this paper. The conclusions drawn are not necessarily those of FMC or IFC.