高效液相色谱-串联质谱法检测三苯乙烯基苯酚聚氧乙烯醚

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。

Determination of tristyrylphenol ethoxylates by high performance liquid chromatography-tandem mass spectrometry

A high performance liquid chromatography-tandem mass spectrometry method for the analysis of tristyrylphenol ethoxylates (TSPnEO) was established. The separation effects of TSPnEO in the four liquid chromatography modes, including reversed-phase liquid chromatography column (XBridge C₁₈, 150 mm×2.1 mm, 3.5 μ m), hydrophilic interaction liquid chromatography column (XBridge HILIC, 150 mm×2.1 mm, 3.5 μ m), amide column (XBridge Amide, 150 mm×2.1 mm, 3.5 μ m) and C₁₈ column (XBridge C₁₈, 50 mm×2.1 mm, 5 μ m) combined with silica column (Nova-Pak Silica, 150 mm×2.1 mm, 4 μ m) were investigated. And the separation effects and sensitivity of TSPnEO in four mobile phases, such as 5 mmol/L ammonium acetate aqueous solution-acetonitrile, 0.1% (v/v) formic acid aqueous solution-acetonitrile, water-acetonitrile and water-methanol, and three eluent gradient conditions were optimized too. The ionization behavior of TSPnEO in electrospray ionization (ESI) was also studied. The results showed that in the ESI positive ion mode, the identified adducts wereM+NH₄]⁺, and the distribution characterization was in Poisson-like distribution. The separation of TSPnEO (n=5-18) was achieved via C₁₈ column combined with the silica column and water-acetonitrile as mobile phases according to the degree of ethoxylation.