用于手性LC-MS分离的柱串联技术可在复杂样品中解析三酰甘油对映异构体和区域异构体，无需流动循环
Column coupling for chiral LC-MS separation resolves triacylglycerol enantiomers and regioisomers in complex samples without flow recycling.
摘要(中文译文)
三酰基甘油（TG）甘油骨架上脂肪酸的位置分布产生了多种区域异构体和立体异构体，它们具有不同的吸收、代谢和组织分布特性。这些脂肪酸中双键位置异构体的存在进一步增加了这种多样性，给分析带来了挑战。为改进对这一众多异构体的测定，我们将手性液相色谱与电喷雾电离高分辨质谱联用。对于对映异构体和区域异构体的分离，我们使用了直链淀粉三（3-氯-4-甲基苯基氨基甲酸酯）固定相（Chiralpak IF-3），并评估了关键色谱参数：流动相组成、柱温和流速。选择乙腈/水（98：2，v/v）作为流动相，在35 °C和0.15 mL/min条件下分离对映异构体和区域异构体。此外，串联三根色谱柱（750 mm）提高了关键对映异构体和区域异构体分离的效率和分辨率。此外，我们的方法能够区分双键位置和顺/反构型不同的TG，这些使用常规反相色谱系统难以分离。该分离方法在肝脏基质中表现出稳定的保留时间和可重复的对映异构体百分比测定。该方法的应用揭示了常规反相色谱无法解析的大鼠肝脏提取物中TG的立体化学多样性。此外，它还能够在暴露于多柔比星后检测对映异构体分布的差异。这凸显了在生物样品中解析TG异构体的重要性。总之，本工作报道了一个稳健的、与质谱兼容的脂质组学手性平台，用于立体特异性TG分析，为未来在立体化学水平上研究脂质重塑和从头脂肪生成提供了分析基础。
Abstract
The positional distribution of fatty acids in the glycerol of triacylglycerols (TGs) gives multiple regioisomeric and enantiomeric species with different absorption, metabolism and tissue distribution. This diversity is further enhanced by the positional isomers of double bonds in these fatty acids which present an analytical challenge. To improve the determination of this plethora of isomers, we coupled chiral liquid chromatography with electrospray ionization high-resolution mass spectrometry. For the separation of enantiomers and regioisomers, we used an amylose tris(3-chloro-4-methylphenylcarbamate) stationary phase (Chiralpak IF-3) and evaluated the key chromatographic parameters: mobile phase composition, column temperature and flow-rate. Acetonitrile/water (98:2, v/v) as mobile phase at 35 °C and 0.15 mL/min was selected for separation of enantiomers and regioisomers. In addition, coupling three columns (750 mm) improved efficiency and resolution for the separation of key enantiomers and regioisomers. In addition, our method discriminated TGs differing in double-bond position and cis/trans configuration, which are difficult to resolve using conventional reversed-phase chromatographic systems. The separation method showed stable retention and reproducible determination of enantiomeric percentages in liver matrices. The application of the method revealed the stereochemical TG diversity in rat liver extracts that is unresolved by conventional RP chromatography. Furthermore, it enabled detection of differences in enantiomeric distribution following exposure to doxorubicin. This highlights the importance of resolving TG isomers in biological samples. In conclusion, this work reports a robust MS-compatible lipidomics chiral platform for stereospecific TG analysis providing an analytical foundation for future investigation of lipid remodelling and de novo lipogenesis at the stereochemical level.
如何引用
AMA
Jenny M Nilsson, David Balgoma, Edvin Dedering Stephansson, Sofia Landström, Curt Pettersson, David Dahlgren, et al. Column coupling for chiral LC-MS separation resolves triacylglycerol enantiomers and regioisomers in complex samples without flow recycling.. Talanta. 2027; doi:10.1016/j.talanta.2026.130202.
APA
Jenny M Nilsson, David Balgoma, Edvin Dedering Stephansson, Sofia Landström, Curt Pettersson, David Dahlgren, et al (2027). Column coupling for chiral LC-MS separation resolves triacylglycerol enantiomers and regioisomers in complex samples without flow recycling.. Talanta. https://doi.org/10.1016/j.talanta.2026.130202
GB/T 7714
Jenny M Nilsson, David Balgoma, Edvin Dedering Stephansson, Sofia Landström, Curt Pettersson, David Dahlgren, et al. Column coupling for chiral LC-MS separation resolves triacylglycerol enantiomers and regioisomers in complex samples without flow recycling.[J]. Talanta, 2027 doi:10.1016/j.talanta.2026.130202.
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