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职业环境中肼的毛细管气相色谱分析
林一民1, 周彬2, 汤利娜2, 王丽娟3, 张稳稳3, 季卫刚3, 杨旭3
1.重庆大学附属肿瘤医院 肿瘤转移与个体化诊治转化研究重庆市重点实验室, 重庆 400030;2.重庆惠能标普科技有限公司, 重庆 401121;3.重庆医药高等专科学校 药学院, 重庆 401331
摘要:
用过量的糠醛衍生转化肼,用质谱对肼的糠醛衍生晶体进行结构定性,对肼糠醛衍生物的晶体、溶剂及肼糠醛衍生物的提取液进行毛细管气相色谱对比分析,获得可靠的定性定量分析信息,优化衍生、萃取和色谱分析等条件,用标准曲线、精密度和准确度试验进行方法评价。实验表明,在糠醛过量的条件下,肼完全转化为2糠醛嗪,保留时间为6.20 min,方法检出下限为0.007 8 mg/L,相对标准偏差2.5%,加标回收率98%~100%。方法的色谱峰形对称、准确、灵敏度高、选择性好,为不同实验室仪器及色谱柱条件下分析检测肼提供了一种快速、准确的条件探索程序。
关键词:    毛细管气相色谱法  糠醛  衍生转化  职业环境
DOI:10.11835/j.issn.1000-582X.2019.12.007
分类号:O657
基金项目:重庆市基础科学与前沿技术研究项目(CSTC2017jcyjAX0446);重庆医药高等专科学校校级课题(ygz2018308)。
Analysis of hydrazine in occupational environment by capillary gas chromatography
LIN Yimin1, ZHOU Bin2, TANG Lina2, WANG Lijuan3, ZHANG Wenwen3, JI Weigang3, YANG Xu3
1.Chongqing Key Laboratory of Translational Research for Cancer Metastasis and Individualized Treatment, Chongqing University Cancer Hospital, Chongqing 400030, P. R. China;2.Chongqing Huinengbiaopu Technology Co. Ltd., Chongqing 401121, P. R. China;3.College of Pharmacy, Chongqing Medical and Pharmaceutical College, Chongqing 401331, P. R. China
Abstract:
Hydrazine is derived with excessive furfural. The crystal of hydrazine derivative conversion is characterized by mass spectrometry. The comparative analyses are made between the hydrazine-derived furfural crystal, solvent, as well as extraction solution of furfural derivatives of hydrazine by the method of capillary gas chromatography. Reliable qualitative and quantitative analytical information is obtained, and the conditions of derivation, extraction and chromatographic analysis are optimized. The method is evaluated by standard curve, precision and accuracy tests. Experiments show that in the case of excessive furfural, hydrazine is completely converted to 2-furaldehyde azine, whose retention time is 6.20 min. The detection limit of the method is 0.007 8 mg/L, the relative standard deviation is 2.5%, and the recovery is in the range of 98% to 100%. The method has the advantages of symmetrical peak shape, high accuracy, high sensitivity and good selectivity. It provides a rapid and accurate procedure for the analysis and determination of hydrazine under different laboratory instruments and chromatographic column conditions.
Key words:  hydrazine  capillary gas chromatography  furfural  derivatization and conversion  occupational environment
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