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建立了高效液相色谱-串联质谱检测三苯乙烯基苯酚聚氧乙烯醚(tristyrylphenol ethoxylates,TSPn EO)的分析方法,并对TSPn EO在反相色谱柱(XBridge C_(18),150 mm×2.1 mm,3.5μm)、亲水相互作用色谱柱(XBridge HILIC,150 m m×2.1 m m,3.5μm)、氨基色谱柱(XBridge Amide,150 m m×2.1 m m,3.5μm)、伪反相色谱柱(C18柱(XBridge C_(18),50 mm×2.1 mm,5μm)与硅胶柱(Nova-Pak Silica,150 mm×2.1 mm,4μm)串联)4种不同液相色谱分离模式下的分离效果进行了研究。实验比较了5 mmol/L乙酸铵水-乙腈、0.1%(v/v)甲酸水-乙腈、水-乙腈和水-甲醇4种流动相组成及3种梯度洗脱条件对分离效果和灵敏度的影响。探讨了TSPnEO在电喷雾离子(ESI)源内的离子化特征,结果表明,在ESI正离子模式下,TSPnEO在离子源内形成[M+NH4]+离子,其聚合度的分布特征符合泊松分布。利用伪反相色谱柱,水-乙腈作为流动相,实现了不同聚合度(n=5~18)TSPnEO的分离。
A high performance liquid chromatography-tandem mass spectrometry (LC-MS / MS) method was developed for the determination of tristyrylphenol ethoxylates (TSPn EO). The analytical method of TSPn EO was performed on a reversed phase column (XBridge C 18, 150 mm × 2.1 (XBridge HILIC, 150 mm × 2.1 mm, 3.5 μm), XBridge Amide (150 mm × 2.1 mm, 3.5 μm), and a pseudo-reversed-phase column The separation efficiency of four different liquid chromatographic separation modes was studied by using column (XBridge C 18, 50 mm × 2.1 mm, 5 μm) and silica gel column (Nova-Pak Silica, 150 mm × 2.1 mm, 4 μm) . The effects of 5 mmol / L ammonium acetate - acetonitrile, 0.1% (v / v) formic acid water - acetonitrile, water - acetonitrile and water - methanol on the mobile phase composition and three gradient elution conditions were compared. influences. The ionization characteristics of TSPnEO in the electrospray ionization (ESI) source were investigated. The results showed that [M + NH4] + ions were formed in the ion source by ESI in the positive mode of ESI. The distribution of the polymerization degree of TSPnEO conforms to the Poisson distribution. The separation of TSPnEO with different polymerization degree (n = 5 ~ 18) was achieved with pseudo-reversed-phase column and water-acetonitrile as mobile phase.