Carrageenans are widely utilized in many commercial applications such as the food and pharmaceutical industry, due to their excellent functional properties. In this study, a sensitive LC-MS/MS method was developed to ...Carrageenans are widely utilized in many commercial applications such as the food and pharmaceutical industry, due to their excellent functional properties. In this study, a sensitive LC-MS/MS method was developed to determine κ-3, κ-5, and κ-7 carrageenan oligosaccharides simultaneously. Optimum MRM transitions for κ-3, κ-5, and κ-7 carrageenan oligosaccharides were(645.079→565.111, [M-H]-),(515.137→474.946, [M-2H]^2-), and(471.484→445, [M-3H]^3-), respectively. Chromatographic separation was performed on an Amide column coupled with a guard column operated at 60℃ under stepwise gradient elution. The linearity of the LC-MS/MS method for κ-3, κ-5, and κ-7 carrageenan oligosaccharides, evaluated over the concentration range of 0.10- 20.0 μmol L^-1, was excellent. The precisions of the method for κ-3, κ-5, and κ-7 carrageenan oligosaccharides were from 0.91% to 9.66%, and the inter-day precisions were from 0.92% to 10.5%. Validation of the LC-MS/MS method indicated that the method was precise and in line with the CFDA guidance. This method has been successfully applied to an in vitro absorption study.展开更多
基金supported by the Shandong Provincial Natural Science Foundation,China (No. ZR2019BC025)Open Research Fund Program of Shandong Provincial Key Laboratory of Glycoscience&Glycotechnology (Ocean University of China)the Fundamental Research Funds for the Central Universities (Nos. 201912008,201964019)。
文摘Carrageenans are widely utilized in many commercial applications such as the food and pharmaceutical industry, due to their excellent functional properties. In this study, a sensitive LC-MS/MS method was developed to determine κ-3, κ-5, and κ-7 carrageenan oligosaccharides simultaneously. Optimum MRM transitions for κ-3, κ-5, and κ-7 carrageenan oligosaccharides were(645.079→565.111, [M-H]-),(515.137→474.946, [M-2H]^2-), and(471.484→445, [M-3H]^3-), respectively. Chromatographic separation was performed on an Amide column coupled with a guard column operated at 60℃ under stepwise gradient elution. The linearity of the LC-MS/MS method for κ-3, κ-5, and κ-7 carrageenan oligosaccharides, evaluated over the concentration range of 0.10- 20.0 μmol L^-1, was excellent. The precisions of the method for κ-3, κ-5, and κ-7 carrageenan oligosaccharides were from 0.91% to 9.66%, and the inter-day precisions were from 0.92% to 10.5%. Validation of the LC-MS/MS method indicated that the method was precise and in line with the CFDA guidance. This method has been successfully applied to an in vitro absorption study.