ANALYTICAL CHEMISTRY
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2020
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IF 6.785
Chengyi Xie,Liancheng Gu,Qidi Wu,Lei Li,Chenlu Wang,Jiancheng Yu,Keqi Tang
Chiral analysis is critical to many research fields due to different biological functions of enantiomers in living systems. Although the use of ion mobility spectrometry (IMS) has become an alternative technology in the area of chiral measurements, there is still a lack of a general chiral selector for IMS-based chiral recognition, especially for small chiral molecules. Here, a new method using oligosaccharides as the chiral selector has been developed to discriminate chiral amino acids (AAs) by trapped ion mobility spectrometry-mass spectrometry (TIMS-MS). We analyzed 21 chiral amino acids, including small molecules (e.g., alanine and cysteine). Our data showed that the use of nonreducing tetrasaccharides was effective for the separation of chiral AAs, which differentiated 21 chiral AAs without using metal ions. By further incorporating a copper ion, the separation resolution could be improved to 1.64 on average, which accounts for an additional 52% improvement on top of the already achieved separation in metal-free analysis. These results indicate that the use of tetrasaccharides is an effective strategy for the separation of AA enantiomers by TIMS. The method developed in this study may open up a new strategy for effective IMS-based chiral analysis.
研究领域:
分析化学
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质谱
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手性
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生物化学
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产品关联
DOI
PubMed
高影响因子
FOOD CHEMISTRY
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2026
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IF 9.8
Xueqian Sun,Ziyu Qu,Di Zhang,Chuan-Fan Ding,Fangling Wu
This study developed a rapid TIMS-MS method combined with computational chemistry to differentiate and quantify three groups of cinnamic acid derivative (CAD) isomers: 2/4- hydroxycinnamic acid (2/4-HCA), α/β-methylcinnamic acid (α/β-MCA), and o/m/p- Methoxycinnamic acid (o/m/p-MCA). Separation leveraged distinct non-covalent complexes formed with α−/β−/γ-cyclodextrin (CDs) and metal ions. Optimal conditions achieved excellent resolution (R p-p up to 1.05), particularly for [2/4-HCA + α-CD + Mg-H] + and [o/m/p-MCA + α-CD + Mg-H] + complexes. Computational analysis confirmed the conformational differences and non-covalent interaction sites enabling separation, aligning well with experiments (error ≤ 3.46%). The method showed high sensitivity of limit of detection (LOD) ≤3.27 ng·mL −1 , linearity (R 2 > 0.99), and successfully quantified CAD isomers in pineapple leaves and cinnamon powder with good recovery (≥80.60%) and precision of relative standard deviation (RSD ≤5.75%). By avoiding chemical derivatization and chromatographic separation, our method provides a rapid and simple platform for the direct analysis of bioactive food components, demonstrating great promise for food quality control.
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DOI
PubMed
高影响因子
ANALYTICAL CHEMISTRY
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2026
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IF 7.3
Simin Zhang,Xiangfeng Chen,Yaping Shi,Xiangyu Zhu,Zongwei Cai
As bioactive compounds, chiral amino acids (AAs) have been demonstrated to play pivotal roles in different physiological processes, thereby influencing human health. The assessment of the relative enantiomeric ratio through analytical methods is essential for indicating the abnormal status of disease progression, which drives the development of effective methods for resolving and identifying enantiomers. This work presents a robust strategy for the ultrahigh-resolution analysis of chiral AAs using MALDI-TIMS-MS. By employing a chiral derivatization process using S-NIFE and stabilizing the soft chain of the derivatization reagent with bimetal ion addition, the separation of 19 pairs of proteinogenic AAs was successfully achieved. This method not only demonstrates outstanding separation capability but also proves its efficiency in determining enantiomeric ratios, extending its applicability to real sample analysis.
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PubMed
高影响因子
ANALYTICAL CHEMISTRY
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2025
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IF 6.7
Naisheng Wu,Fangling Wu,Sisi He,Jia Wang,Huiqing Ding,Chuan-Fan Ding
This study presents a novel approach for the rapid and high-resolution separation of estrogen isomers (α/β-estradiol and estriol: α/β-E2/E3) using trapped ion mobility mass spectrometry (TIMS-MS). Systematically, evaluating cyclodextrin (α-, β-, and γ-CD) as separation reagents and exploring metal ions as coordinating ligands, we achieved enhanced isomer differentiation, in which the separation resolution (RP–P) was increased from 0.204 to 1.533. Density functional theory (DFT) calculations and noncovalent interaction visualization analysis provided molecular-level insights into the structural and interaction differences driving these separations, highlighting the critical roles of host–guest interactions and metal coordination geometry. Additionally, quantitative analysis and method validation for the estrogen isomers were measured, with a good linearity of R2 value higher than 0.99 and RSD ≤ 2.28%. Finally, the method was applied to detect and quantify α/β-E2/E3 in human urine samples; good recoveries of ≥79.78% were obtained with RSD ≤ 4.35% for intraday and RSD ≤ 9.56% for interday. The combined experimental and theoretical results demonstrate the potential of this TIMS-MS-based strategy for clinical diagnostics and bioanalytical applications requiring precise estrogen isomer separation.
研究领域:
分析化学
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分子生物学
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生物分析化学
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临床检验医学
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代谢组学
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药物代谢
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质谱技术
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产品关联
DOI
PubMed
高影响因子
TALANTA
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2021
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IF 6.057
Pengfei Guan,Chengyi Xie,Lei Li,Xiangyu Fang,Fangling Wu,Jun Jack Hu,Keqi Tang
Carbohydrates are an indispensable part of early life evolution. The determination of their structures is a key step to analyze their critical roles in biological systems. A variation of composition , glycosidic linkage , and (or) configuration between carbohydrate isomers induces structure diversity and brings challenges for their structural determination. Ion mobility spectrometry (IMS), an emerging gas-phase ion separation technology, has been considered as a promising tool for performing carbohydrate structure elucidation . In this work, eight disaccharides were analyzed by trapped ion mobility spectrometry-mass spectrometry (TIMS-MS) in the negative ion mode as the complexed form of [M + X] - , where M = disaccharide, and X = Cl, Br, and I. As compared to the positive ion analysis of the selected disaccharide in a sodiated form, a reversal charge state provided the ability to eliminate or even reverse the collision cross section (CCS) difference between disaccharide isomers. By the combination of TIMS analysis and the calculation of density functional theory, the only observed two conformers of ions [lactulose + I] - may result from different adduction sites for an iodide anion. Based on the comparison of different halogen adducts, the [M + I] - ion form exhibited more powerful ability for isomeric disaccharide differentiation with an average resolution ( R P-P ) of 1.17, which results in a 34.5% improvement as compared to the corresponding chloride adducts. This result indicates that the use of negative charge states, especially the complexation of an iodide anion, could be a supplemental strategy to commonly used positive ion analysis for carbohydrate separation.
研究领域:
分析化学
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质谱
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碳水化合物化学
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离子迁移率光谱
✓ 已验证
产品关联
DOI
PubMed
高影响因子
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