论文部分内容阅读
采用高效液相色谱-四极杆/静电场轨道阱高分辨率质谱(HPLC-Q/Orbitrap MS)建立了寡糖轮廓分析的方法。通过对纯天然蜂蜜和淀粉类糖浆中的麦芽三糖、麦芽四糖、麦芽五糖、麦芽六糖和麦芽七糖进行定性定量分析,发现淀粉类糖浆中含有未被酶解完全的微量麦芽类寡糖,且麦芽七糖在所有检测样本中干扰小,对结果的定量无影响,而其他寡糖类物质的定性和定量结果会存在干扰。最终选择麦芽七糖作为蜂蜜中掺入淀粉糖浆的典型标志物。在实际样品分析中,根据麦芽七糖的保留时间和离子对的相对丰度比可以定性判断蜂蜜中是否掺有淀粉糖浆;通过标准曲线法可以定量测定样液中麦芽七糖的含量。在20,50,100 mg/kg 3个加标水平下,麦芽七糖的平均回收率为75%~82%,相对标准偏差(RSD,n=5)为3.1%~6.7%,方法检出限为0.1μg/m L。应用该方法可在10 min内完成整个分析过程,且样品前处理简单,结果可靠,灵敏度高,可用于纯天然蜂蜜中掺入淀粉糖浆的快速确证和检测。
A method for the profile analysis of oligosaccharides was established by high performance liquid chromatography-quadrupole / electrostatic field orbitrap high-resolution mass spectrometry (HPLC-Q / Orbitrap MS). Qualitative and quantitative analysis of maltotriose, maltotetraose, maltotetraose, maltohexaose and maltoheptaose in pure natural honey and starchy syrup found that the starchy syrup contained trace amounts of malt without complete enzymolysis Oligosaccharides, and maltoheptaose in all the test sample interference is small, the results have no effect on the quantitative, and other oligosaccharides qualitative and quantitative results will interfere. Maltotriose was finally chosen as a typical marker for the incorporation of starch syrup in honey. In the actual sample analysis, according to the retention time of maltoheptaose and the relative abundance ratio of ion pair, it can be qualitatively determined whether the starch is mixed with the starch syrup. The content of maltoheptaose in the sample solution can be quantitatively determined by the standard curve method. The average recoveries of maltoheptaose ranged from 75% to 82% and the relative standard deviations (RSD, n = 5) ranged from 3.1% to 6.7% at the three spiked levels of 20, 50 and 100 mg / kg. 0.1 μg / m L. The method can be used in 10 minutes to complete the entire analysis process, and the sample pretreatment is simple, reliable results, high sensitivity, can be used for rapid confirmation and testing of natural honey mixed with starch syrup.