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A Sensitive Ultra-High Performance Liquid Chromatography–Tandem Mass Spectrometry Method Based on Derivatization with 1-Nitro-2-Naphthaldehyde for Determination of Alkylhydrazines in Surface Water
Journal of AOAC INTERNATIONAL ( IF 1.6 ) Pub Date : 2021-09-14 , DOI: 10.1093/jaoacint/qsab112
Jin-Ah Oh 1 , Ho-Sang Shin 2 , Hyun-Hee Lim 3
Affiliation  

Background Alkylhydrazines are widely used in industrial fields. An analysis of alkylhydrazines in surface water is needed because these chemicals are likely to be discharged into wastewater and enter aquatic environments. Objective An ultra-high performance liquid chromatography (UHPLC)–tandem mass spectrometry (MS/MS) method was developed to determine the levels of five alkylhydrazines (N, N-dimethylhydrazine, ethylhydrazine, 1-isopropylhydrazine, phenylhydrazine, and 1-methyl-1-phenylhydrazine) in surface water. Methods This method is based on the derivatization of alkylhydrazines with 1-nitro-2-naphthaldehyde (NNA) in water. A derivatization reagent dosage of 0.5 mg NNA, a pH of 2, and a reaction time of 30 min at 40°C were determined to be the optimal conditions for UHPLC–MS/MS detection. The derivatives were injected into the LC system without additional extraction or purification steps. Results The proposed method was used under optimized conditions to detect alkylhydrazines in surface water, with the limit of quantification found to be 0.01–0.03 μg/L. The accuracy ranged from 91.0 to 106.0%, and the precision, expressed as the relative standard deviation, was less than 10%. Of the five alkylhydrazines, only N, N-dimethyl hydrazine was detected in the real samples at a concentration range of 0.010–0.041 μg/L. Conclusion The developed method can be used to confirm the presence of alkylhydrazine residues in surface water and represents an important tool for evaluating the fate of alkylhydrazines in surface water. Highlights A UHPLC-MSMS method was developed in order to dtermine the alkylhydrazine in surface water after derivatization without an extraction or cleanup step.

中文翻译:

基于1-硝基-2-萘醛衍生的灵敏超高效液相色谱-串联质谱法测定地表水中的烷基肼

背景烷基肼广泛用于工业领域。需要对地表水中的烷基肼进行分析,因为这些化学物质可能会排放到废水中并进入水生环境。目的 建立超高效液相色谱(UHPLC)-串联质谱(MS/MS)方法测定五种烷基肼(N,N-二甲基肼、乙基肼、1-异丙基肼、苯肼和1-甲基肼)的含量。 1-苯肼)在地表水中。方法 该方法基于烷基肼与 1-硝基-2-萘醛 (NNA) 在水中的衍生化反应。0.5 mg NNA 的衍生化试剂剂量、2 的 pH 值和 40°C 下 30 分钟的反应时间被确定为 UHPLC-MS/MS 检测的最佳条件。衍生物无需额外的萃取或纯化步骤即可注入 LC 系统。结果本方法在优化条件下用于地表水中烷基肼的检测,定量限为0.01~0.03 μg/L。准确度范围为91.0~106.0%,以相对标准偏差表示的精密度小于10%。在五种烷基肼中,仅在实际样品中检测到 N,N-二甲基肼,浓度范围为 0.010–0.041 μg/L。结论 所开发的方法可用于确认地表水中烷基肼残留的存在,是评估地表水中烷基肼归宿的重要工具。
更新日期:2021-09-14
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