Yu-Hsuan Tsai , Chia-Wei Tsai , Christopher A. Tipple
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引用次数: 2
摘要
采用液相色谱-质谱法对11种糖和糖醇进行了分析。建立了一种糖和糖醇的分离方法，重点研究了山梨醇/甘露醇异构体对的分离。对该方法进行了检出限、稳定性、干扰、电离抑制等方面的研究。麦芽糖醇的检出限为9.2 × 10-3 mM，红细胞的检出限为2.3 mM (3.2 ppm至2.8 × 102 ppm)。对糖和糖醇在低浓度和高浓度下的稳定性进行了5天的测试。大多数糖在高浓度下至少稳定两天，而6个糖在低浓度下稳定，表明需要及时分析。干扰研究是在存在硝化糖的情况下进行的，这可能存在于该方法的法医应用中。甘露醇己酸酯(MHN)和四硝酸赤藓糖醇(ETN)均无干扰。最后，对样品采集基质抑制或增强糖和糖醇分析信号的潜力进行了评价。除果糖外，任何分析物在高或低浓度下均未观察到显著的增强/抑制。对法医样本进行了实地试验，证明了该程序的潜力。该方法成功地用于分析六个爆炸后样品，结果表明其中五个样品中至少存在一种糖/糖醇。
A validated method for the analysis of sugars and sugar alcohols related to explosives via liquid chromatography mass spectrometry (LC-MS) with post-column addition
The analysis of eleven sugars and sugar alcohols was performed via liquid chromatography with mass spectrometric detection. A method for the separation of the sugars and sugar alcohols, with the specific emphasis on the separation of the isomeric pair sorbitol/mannitol, was developed. The method was validated, with the following studies included: limit of detection, stability, interference, and ionization suppression. The limits of detection ranged from 9.2x10-3 mM for maltitol up to 2.3 mM for erythrose (3.2 ppm up to 2.8 x102 ppm). The sugars and sugar alcohols were tested at low and high concentrations over 5 days for their stability. Most of the sugars were stable for at least two days at the high concentration, while 6 were stable at the low concentration indicating the need to analyze promptly. An interference study was conducted with nitrated sugars present, which may be present in the forensic application for which the method is intended. There was no interference observed from either mannitol hexanitrate (MHN) or erythritol tetranitrate (ETN). Finally, the effect of a sample collection matrix was evaluated for its potential to either suppress or enhance the analytical signal from the sugars and sugar alcohols. There was no significant enhancement/suppression observed, at high or low concentration, for any analyte except fructose. A field trial was made of forensic samples which demonstrated the potential of the procedure. The method was successfully used for the analysis of six post-blast samples, which indicated the presence of at least one sugar/sugar alcohol in five of those samples.
期刊介绍：
Forensic Chemistry publishes high quality manuscripts focusing on the theory, research and application of any chemical science to forensic analysis. The scope of the journal includes fundamental advancements that result in a better understanding of the evidentiary significance derived from the physical and chemical analysis of materials. The scope of Forensic Chemistry will also include the application and or development of any molecular and atomic spectrochemical technique, electrochemical techniques, sensors, surface characterization techniques, mass spectrometry, nuclear magnetic resonance, chemometrics and statistics, and separation sciences (e.g. chromatography) that provide insight into the forensic analysis of materials. Evidential topics of interest to the journal include, but are not limited to, fingerprint analysis, drug analysis, ignitable liquid residue analysis, explosives detection and analysis, the characterization and comparison of trace evidence (glass, fibers, paints and polymers, tapes, soils and other materials), ink and paper analysis, gunshot residue analysis, synthetic pathways for drugs, toxicology and the analysis and chemistry associated with the components of fingermarks. The journal is particularly interested in receiving manuscripts that report advances in the forensic interpretation of chemical evidence. Technology Readiness Level: When submitting an article to Forensic Chemistry, all authors will be asked to self-assign a Technology Readiness Level (TRL) to their article. The purpose of the TRL system is to help readers understand the level of maturity of an idea or method, to help track the evolution of readiness of a given technique or method, and to help filter published articles by the expected ease of implementation in an operation setting within a crime lab.
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