CAJ | 학술논문

建立了高效液相色谱-四极杆／静电场轨道阱高分辨质谱法测定奶粉中低聚果糖的方法。奶粉样品用水溶解，加乙酸锌沉淀蛋白，经离心、0.22μm 粒径的微孔膜过滤后，采用 Carbohydrate 色谱柱（100 mm ×2.1 mm，2.6μm）进行分离，以乙腈与0.1％乙酸水溶液为流动相进行梯度洗脱。质谱采用正离子 Target-MS／MS 模式，在分离窗口为 m／z 4.0和碰撞能为30 eV的条件下，提取响应值较高且在待测样品中无干扰的目标子离子的精确质量数，此方法能够很好地排除样品中的基质干扰。在所建立的色谱-质谱条件下，蔗果三糖（GF2）、蔗果四糖（GF3）和蔗果五糖（GF4）能够得到较好的分离，高分辨质谱提取的质量准确度小于5×10－6（5 ppm），整个分析时间只需10 min。该方法对 GF2和 GF3的检出限可达100μg／kg，对 GF4的检出限可达55μg／kg。待测物质采用外标法定量，线性关系良好，相关系数均大于0.998。通过加标验证，在5、10和20 mg／kg 3个加标水平下，奶粉中 GF2、GF3和 GF4的平均回收率在75.8％~107.3％范围内，相对标准偏差（ RSD）在1.6％~8.3％范围内。该方法样品前处理过程简单，只需沉淀蛋白质，通过二级子离子的选择即可排除基质干扰，分析时间短，测定结果准确、可靠，适用于任何奶粉的高通量测定。
건립료고효액상색보-사겁간／정전장궤도정고분변질보법측정내분중저취과당적방법。내분양품용수용해，가을산자침정단백，경리심、0.22μm 립경적미공막과려후，채용 Carbohydrate 색보주（100 mm ×2.1 mm，2.6μm）진행분리，이을정여0.1％을산수용액위류동상진행제도세탈。질보채용정리자 Target-MS／MS 모식，재분리창구위 m／z 4.0화팽당능위30 eV적조건하，제취향응치교고차재대측양품중무간우적목표자리자적정학질량수，차방법능구흔호지배제양품중적기질간우。재소건립적색보-질보조건하，자과삼당（GF2）、자과사당（GF3）화자과오당（GF4）능구득도교호적분리，고분변질보제취적질량준학도소우5×10－6（5 ppm），정개분석시간지수10 min。해방법대 GF2화 GF3적검출한가체100μg／kg，대 GF4적검출한가체55μg／kg。대측물질채용외표법정량，선성관계량호，상관계수균대우0.998。통과가표험증，재5、10화20 mg／kg 3개가표수평하，내분중 GF2、GF3화 GF4적평균회수솔재75.8％~107.3％범위내，상대표준편차（ RSD）재1.6％~8.3％범위내。해방법양품전처리과정간단，지수침정단백질，통과이급자리자적선택즉가배제기질간우，분석시간단，측정결과준학、가고，괄용우임하내분적고통량측정。
A method of high performance liquid chromatography-quadrupole/electrostatic field Orbitrap high resolution mass spectrometry( HPLC-Q/Orbitrap MS ) was developed to deter-mine fructo-oligosaccharides in milk powder. The milk powder samples were dissolved in deion-ized 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 acetoni-trile 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 accu-rate 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 correla-tion 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.