Sørensen Lambert K
Steins Laboratorium, Blomstervej 1, 8381 Tilst, Denmark.
Rapid Commun Mass Spectrom. 2006;20(24):3625-33. doi: 10.1002/rcm.2775.
A liquid chromatographic/tandem mass spectrometric method using pneumatically assisted electrospray ionisation (LC/ESI-MS/MS) was developed for the determination of gangliosides GD3 and GM3 in milk and infant formulae. The gangliosides were extracted in a chloroform/methanol/water environment and cleaned up by solid-phase extraction (SPE) on an end-capped C8 sorbent. The gangliosides were detected in negative ion mode after separation on a reversed-phase (RP) C5 analytical column. From the different ganglioside molecular species, product ions at m/z 290 corresponding to an N-acetylneuraminic acid fragment were produced in the collision cell and used in selected reaction monitoring. A standard addition technique was applied for quantification. The relative repeatability standard deviations were less than 5% for GD3 (level 10 mg/L) and 14% for GM3 (level 0.1-0.2 mg/L).
建立了一种采用气动辅助电喷雾电离的液相色谱/串联质谱法(LC/ESI-MS/MS),用于测定牛奶和婴儿配方奶粉中的神经节苷脂GD3和GM3。神经节苷脂在氯仿/甲醇/水环境中萃取,并通过在封端C8吸附剂上进行固相萃取(SPE)进行净化。在反相(RP)C5分析柱上分离后,以负离子模式检测神经节苷脂。在不同的神经节苷脂分子种类中,碰撞池中产生了对应于N-乙酰神经氨酸片段的m/z 290的产物离子,并用于选择反应监测。采用标准加入法进行定量。GD3(浓度为10 mg/L)的相对重复性标准偏差小于5%,GM3(浓度为0.1 - 0.2 mg/L)的相对重复性标准偏差小于14%。