Citation: LIU Yun, DING Tao, XU Suli, WU Bin, SHEN Chongyu, ZHANG Rui, WANG Yan, FEI Xiaoqing. Determination of fructo-oligosaccharides in milk powder by high performance liquid chromatography- quadrupole/electrostatic field orbitrap high resolution mass spectrometry[J]. Chinese Journal of Chromatography, ;2015, 33(10): 1040-1045. doi: 10.3724/SP.J.1123.2015.06010 shu

Determination of fructo-oligosaccharides in milk powder by high performance liquid chromatography- quadrupole/electrostatic field orbitrap high resolution mass spectrometry

LIU Yun ¹ ,
DING Tao ^1,, ,
XU Suli ² ,
WU Bin ¹ ,
SHEN Chongyu ¹ ,
ZHANG Rui ¹ ,
WANG Yan ¹ ,
FEI Xiaoqing ¹

1.
1. Animal, Plant and Food Inspection Center, Jiangsu Entry-Exit Inspection and Quarantine Bureau, Nanjing 210001, China;

Corresponding author: DING Tao,
Received Date: 8 June 2015

Fund Project: 江苏出入境检验检疫局科技计划项目(2015KJ29) (2015KJ29)国家科技支撑计划课题(2014BAK19B00,2014BAK19B02). (2014BAK19B00,2014BAK19B02)

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 μm. The analytes were separated on a Carbohydrate column (100 mm×2.1 mm, 2.6 μm) 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-β-fructofuranosyl nystose (GF₄) were well separated and the accuracy of extracted mass routinely detected was below 5×10^-6 (5 ppm). The whole analysis time is only ten minutes. The detection limits for GF₂ and GF₃ were 100 μg/kg, and the detection limit for GF₄ was 55 μg/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.
1. [1]
  [1] Zhang W. Journal of Biological (张伟. 生物学杂志), 2000, 17(1): 7
2. [2]
  [2] Jiang B, Zhang T, Wang Z. Journal of Wuxi University for Light Industry (江波, 张涛, 王璋. 无锡轻工大学学报), 2001, 20(5): 445
3. [3]
  [3] Chen M X, Zhu W J. Biology Teaching (陈木香, 朱文杰. 生物学教学), 2008, 33(5): 61
4. [4]
  [4] Liu Y F, Li D, Tang H C, et al. Journal of Dairy Science and Technology (刘玉峰, 李东, 唐华澄, 等. 乳业科学与技术), 2012, 35(1): 40
5. [5]
  [5] Gnoth M J, Kunz C, Kinne-Saffran E, et al. J Nutr, 2000, 130(12): 3014
6. [6]
  [6] Gao X J. Liquor Making (高晓娟. 酿酒), 2008, 35(4): 90
7. [7]
  [7] GB 2760-2007
8. [8]
  [8] Robefrorid M B. Am J Clin Nutr, 2001, 73(Suppl): 406
9. [9]
  [9] Geng L J, Huang J R, Feng F, et al. Chinese Journal of Chromatography (耿丽娟, 黄峻榕, 冯峰, 等. 色谱), 2014, 32(12): 1380
10. [10]
  [10] AOAC Official Method 997.08
11. [11]
  [11] Wei F, Wu Z Y, Ma L Y, et al. Asia Pacific Traditional Medicine (魏锋, 吴朝阳, 马玲云, 等. 亚太传统医药), 2009, 5(9): 20
12. [12]
  [12] Ding H L, Li C, Jin P, et al. Chinese Journal of Chromatography (丁洪流, 李灿, 金萍, 等. 色谱), 2013, 31(8): 804
13. [13]
  [13] Wang Y Z, Yao P J, Wei Y A. Food Industry (王银珍, 姚评佳, 魏远安. 食品工业), 2009(2): 71
14. [14]
  [14] Lin S J, Xiao H L, Guo B K. Chinese Journal of Health Inspection (林赛君, 肖海龙, 郭柏坤. 中国卫生检验杂志), 2009, 19(11): 2549
15. [15]
  [15] Wang M H, Li M, Guo J, et al. Chinese Journal of Health Inspection (王美菡, 李敏, 郭健, 等. 中国卫生检验杂志), 2007, 17(6): 961
16. [16]
  [16] Zhang Y Y, Nie S P, Wan C, et al. Food Science (张媛媛, 聂少平, 万成, 等. 食品科学), 2009, 30(18): 237
17. [17]
  [17] Bai J, Jiang J D, Tao D L. Food Science (白靖, 姜金斗, 陶大利. 食品科学), 2014, 35(2): 257
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