Yang Fang-Chao, Yang Yang, Yan Long, Wang Feng-Yun, Wu Lei, Xia Ming-Zhu, Li Xiao-Sen
School of Chemistry and Chemical Engineering, Nanjing University of Sciences & Technology Nanjing 210094 P. R. China
State Key Laboratory of NBC Protection for Civilian Beijing 102205 China
RSC Adv. 2023 Sep 14;13(39):27535-27548. doi: 10.1039/d3ra04697d. eCollection 2023 Sep 8.
Methyl-diethanolamine (CAS: 105-59-9), ethyl-diethanolamine (CAS: 139-87-7), and triethanolamine (CAS: 102-71-6) were identified as the degradation products and bio-markers of nitrogen mustard exposure. Sensitive and convenient detection methods for amino alcohol are of great importance to identify nitrogen mustard exposure in forensic analysis. Herein, analytical methods including gas chromatography-tandem mass spectrometry combined with heptafluorobutyryl derivatization and solid phase extraction were established for retrospective detection of the biomarkers in human plasma and urine samples. The efficiency of the method was improved by optimizing the conditions for sample preparation and the GC-MS/MS method. The optimization included the derivatization temperature, reaction time, reagent dosage and solid phase extraction cartridges, eluent and pH of the loading sample. The results indicated that the SCX cartridge resulted in better enrichment and purification effects, and the best recovery could be obtained with pH = 3-4 for the loading samples and an eluent of 2 mL 10% NHOH/MeOH. The GC-MS/MS parameters were also optimized for better specificity and sensitivity. The established method was fully validated for each analyte both in plasma and urine matrixes. The linear range of analytes in plasma was 1.0-1000 ng mL with a correlation parameter () of ≥0.994, intra-day/inter-day accuracy of 93.7-117%, and relative standard deviation (RSD) of ≤6.5%. Meanwhile the results in urine were 1.0-1000 ng mL with of ≥0.996, intra-day/inter-day accuracy of 94.3-122%, and RSD of ≤6.6%. The detection limit of the analytes was 1.0 ng mL. The method was applied for the detection and identification of trace amino alcohols present in urine samples dispatched by the Organization for the Prohibition of Chemical Weapons (OPCW) and the results were confirmed to be correct.
甲基二乙醇胺（CAS：105 - 59 - 9）、乙基二乙醇胺（CAS：139 - 87 - 7）和三乙醇胺（CAS：102 - 71 - 6）被确定为氮芥暴露的降解产物和生物标志物。对氨基醇进行灵敏且便捷的检测方法对于法医分析中识别氮芥暴露至关重要。在此，建立了包括气相色谱 - 串联质谱联用七氟丁酰衍生化和固相萃取的分析方法，用于回顾性检测人血浆和尿液样本中的生物标志物。通过优化样品制备条件和气相色谱 - 串联质谱方法提高了该方法的效率。优化内容包括衍生化温度、反应时间、试剂用量以及固相萃取柱、洗脱液和上样样品的pH值。结果表明，强阳离子交换（SCX）柱具有更好的富集和净化效果，当上样样品pH = 3 - 4且洗脱液为2 mL 10%氢氧化铵/甲醇时可获得最佳回收率。还对气相色谱 - 串联质谱参数进行了优化以提高特异性和灵敏度。所建立的方法在血浆和尿液基质中对每种分析物都进行了充分验证。血浆中分析物的线性范围为1.0 - 1000 ng/mL，相关系数（r）≥0.994，日内/日间准确度为93.7 - 117%，相对标准偏差（RSD）≤6.5%。同时尿液中的结果为1.0 - 1000 ng/mL，r≥0.996，日内/日间准确度为94.3 - 122%，RSD≤6.6%。分析物的检测限为1.0 ng/mL。该方法应用于禁止化学武器组织（OPCW）送检的尿液样本中痕量氨基醇的检测和鉴定，结果经证实是正确的。
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