PMID- 26930960 OWN - NLM STAT- MEDLINE DCOM- 20160426 LR - 20190923 IS - 1000-8713 (Print) IS - 1000-8713 (Linking) VI - 33 IP - 10 DP - 2015 Oct TI - [Determination of fructo-oligosaccharides in milk powder by high performance liquid chromatography-quadrupole/electrostatic field orbitrap high resolution mass spectrometry]. PG - 1040-5 AB - A method of high performance liquid chromatography-quadrupole/electrostatic field Orbitrap high resolution mass spectrometry (HPLC-Q/Orbitrap MS) was developed to determine fructo-oligosaccharides in milk powder. The milk powder samples were dissolved in deionized water. Subsequently, an aqueous solution of zinc acetate was used to precipitate protein. After centrifugation, the final aqueous solution was filtered by a polytetrafluoroethylene (PTFE) membrane with pore size of 0.22 mum. The analytes were separated on a Carbohydrate column (100 mm x 2.1 mm, 2.6 mum) through gradient elution with the combination of acetonitrile and 0.1% formic acid aqueous solution. The target-MS/MS templates were performed at isolation window of m/z 4.0 and collision energy of 30 eV in positive mode to extract the accurate product ion mass of analytes. Under the optimal condition, 1-kestose (GF2), nystose (GF3) and 1-F-beta-fructofuranosyl nystose (GF4) were well separated and the accuracy of extracted mass routinely detected was below 5 x 10(-6) (5 ppm). The whole analysis time is only ten minutes. The detection limits for GF2 and GF3 were 100 mug/kg, and the detection limit for GF4 was 55 mug/kg. Good linearities were obtained in their respective linear ranges with correlation coefficients higher than 0.998. The average recoveries at three spiked levels (5, 10 and 20 mg/kg) were in the range of 75.8%-107.3% and the relative standard deviations (RSDs) were in the range of 1.6% - 8.3%. The proposed method is simple, sensitive, fast and only in need of precipitation of proteins. The interference of matrix can be eliminated through the selection of product ion. The results were convenient and reliable and thus can be used in the large batch determination of any milk powder. FAU - Liu, Yun AU - Liu Y FAU - Ding, Tao AU - Ding T FAU - Xu, Suli AU - Xu S FAU - Wu, Bin AU - Wu B FAU - Shen, Chongyu AU - Shen C FAU - Zhang, Rui AU - Zhang R FAU - Wang, Yan AU - Wang Y FAU - Fei, Xiaoqing AU - Fei X LA - chi PT - Journal Article PL - China TA - Se Pu JT - Se pu = Chinese journal of chromatography JID - 9424804 RN - 0 (Oligosaccharides) RN - 0 (fructooligosaccharide) SB - IM MH - Animals MH - Chromatography, High Pressure Liquid MH - Milk/*chemistry MH - Oligosaccharides/*analysis MH - Tandem Mass Spectrometry EDAT- 2016/03/05 06:00 MHDA- 2016/04/27 06:00 CRDT- 2016/03/03 06:00 PHST- 2016/03/03 06:00 [entrez] PHST- 2016/03/05 06:00 [pubmed] PHST- 2016/04/27 06:00 [medline] AID - 10.3724/sp.j.1123.2015.06010 [doi] PST - ppublish SO - Se Pu. 2015 Oct;33(10):1040-5. doi: 10.3724/sp.j.1123.2015.06010.