首页> 外文期刊>Journal of separation science. >Determination of disialoganglioside GD3 and monosialoganglioside GM3 in infant formulas and whey protein concentrates by ultra-performance liquid chromatography/electrospray ionization tandem mass spectrometry
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Determination of disialoganglioside GD3 and monosialoganglioside GM3 in infant formulas and whey protein concentrates by ultra-performance liquid chromatography/electrospray ionization tandem mass spectrometry

机译:超高效液相色谱/电喷雾串联质谱法测定婴儿配方奶粉和乳清蛋白浓缩物中的双唾液酸神经节苷脂GD3和单唾液酸神经节苷脂GM3

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摘要

A method of ultra-performance liquid chromatography combined with electrospray ionization triple quadrupole tandem mass spectrometry (UPLC-ESI-MS/MS) has been established for simultaneous determination of major disialoganglioside 3 (GD3) and monosialoganglioside 3 (GM3) in infant formulas and whey protein concentrates. Gangliosides were extracted by using the technique of Svennerholm and Fredman and then cleaned up with OASIS HLB solid-phase extraction (SPE) cartridges. The various molecular species of gangliosides were separated on an Acquity UPLC BEH C8 column and analyzed under the negative ion mode. GD3 and GM3 were rapidly quantified using internal standard (IS) method. The developed method was further validated by determining the linearity, average recovery, sensitivity (limit of quantification), and precision. The results presented high correlation coefficients (R ~2 < 0.993) of the selected 16 gangliosides molecular species and provided the respective linear ranges. The limit of quantification was 0.325-0.734 mg/100 g for eight molecular species of GD3 and 0.008-0.312 mg/100 g for eight molecular species of GM3, respectively. The reasonable average recoveries (81-95%) and precision (relative standard deviation [RSD] ≥15%) were also demonstrated in three different spiked levels. This new method would be very useful in the quantitative determination of gangliosides in infant formulas and whey protein concentrates.
机译:建立了一种高效液相色谱结合电喷雾电离三重四极杆串联质谱(UPLC-ESI-MS / MS)的方法,用于同时测定婴儿配方奶粉和乳清中的主要去唾液酸神经节苷脂3(GD3)和单唾液酸神经节苷脂3(GM3)。蛋白质浓缩物。使用Svennerholm和Fredman的技术提取神经节苷脂,然后用OASIS HLB固相萃取(SPE)柱进行净化。在Acquity UPLC BEH C8色谱柱上分离神经节苷脂的各种分子,并在负离子模式下进行分析。 GD3和GM3使用内标(IS)方法快速定量。通过确定线性,平均回收率,灵敏度(定量限)和精密度进一步验证了开发的方法。结果显示所选的16种神经节苷脂分子种类具有较高的相关系数(R〜2 <0.993),并提供了各自的线性范围。八种分子GD3的定量限分别为0.325-0.734 mg / 100 g和八种分子GM3的定量限为0.008-0.312 mg / 100 g。在三个不同的加标水平上也显示了合理的平均回收率(81-95%)和精密度(相对标准偏差[RSD]≥15%)。该新方法在婴儿配方食品和乳清蛋白浓缩物中神经节苷脂的定量测定中非常有用。

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