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市政污水中苯丙胺和甲基苯丙胺衍生化测定应用研究

Study on Determination of Derivatization of Amphetamine and Methamphetamine in Municipal Wastewater

【作者】 孙鹏

【导师】 王德高; 杨萌;

【作者基本信息】 大连海事大学 , 工程硕士(专业学位), 2017, 硕士

【摘要】 苯丙胺和甲基苯丙胺是两种代表性的对中枢神经系统具有显著兴奋作用的兴奋剂,其中甲基苯丙胺已经成为我国主要的滥用毒品。由于毒品滥用的非法性和低流行性,传统调查方法较难获取毒品滥用量真实数据。近年来基于市政污水药物残留分析的污水流行病学方法在毒品滥用调查方面展现出巨大的优势。污水流行病学方法的基础就是对市政污水中的药物残留进行分析。由于苯丙胺和甲基苯丙胺物质分子结构含有氨基官能团,极性较大,易与色谱固定相形成氢键,直接进行气相色谱分析,会导致峰形拖尾,检测灵敏度较差。本论文研究了使用气相色谱质谱方法测定污水中苯丙胺和甲基苯丙胺衍生化产物的方法。针对污水中药物残留极性大和浓度低的特点,分别使用七氟丁酸酐和三氟乙酸酐对两种物质进行衍生化,并对衍生化条件进行优化。七氟丁酸酐衍生化条件可以设置为温度50℃、时间50 min、反应剂量20 μL和碱液洗涤的方法。三氟乙酸酐衍生化条件可以设置为温度50℃、时间30 min和反应剂量25 μL以及碱洗。通过对比相同质量的苯丙胺和甲基苯丙胺衍生化效果,发现三氟乙酸酐比七氟丁酸酐获得更低的检测限和更高的处理效率,因此在测定实际样品中使用三氟乙酸酐进行衍生化。通过对实际污水样品分析发现,大连市11个污水处理厂进水样品中甲基苯丙胺和苯丙胺浓度范围分别为35.9~696 ng/L和2.75~12.9 ng/L。根据人口数量、污水流量和甲基苯丙胺代谢比例等因素,计算每个污水处理厂服务区域的人均滥用量范围为9~923 μg/d。2015年11月和2016年的8月两个月时间范围内,大连市成年人群(15-64岁)甲基苯丙胺的流行率为0.65%~1.48%。通过本研究结果表明基于污水分析的污水流行病学方法可以较为快速得到一个地区的甲基苯丙胺滥用量的实时数据,为公安禁毒部门提供实时毒品滥用数据。

【Abstract】 Amphetamine and methamphetamine are two kinds of stimulants that have significant stimulating effects on the central nervous system,and methamphetamine has become the main illicit drug in China.Because of the illegality and low prevalence of drug abuse,the traditional investigation are difficult to obtain and drug abuse among general population.In recent years,sewage epidemiology has shown great advantages in the investigation of drug abuse.The basis of sewage epidemiology is the analysis of drug residues in municipal wastewater.However,amphetamine and methamphetamine containing amino groups can form the hydrogen bonds with the stationary phase in gas chromatography,which will lead to the poor sensitivity and peak tailing.In this paper,derivatization and gas chromatography-mass spectrometry were used to determine amphetamine and methamphetamine in wastewater.Amphetamine and methamphetamine were derivatized with trifluoroacetic anhydrid(TFA)and heptafluorobutyric anhydride(HBFA),and the derivatization conditions were optimized.The conditions for the derivation of HBFA can be set at temperatures of 50 ℃,time 50 min,dose of 20 μL and lye washing.Three acetic anhydride derivatization conditions can be set at 50℃,30 min and reaction dose of 25 μL.Comparision with HBFA,TFA has the best derivatization effect with lower detection limit and higher processing efficiency.Through the analysis of actual wastewater samples with TFA,it was found that the average concentrations of methamphetamine and amphetamine in influent of 11 sewage treatment plants in Dalian ranged from 35.9~696 ng/L and 2.75~12.9 ng/L,respectively.According to the population,the flow rate and the metabolic proportion of methamphetamine,the amount of abuse per capita is 9~923 μg/d.The prevalence of methamphetamine among adults(15-64 years old)in Dalian was 0.65%~1.48%.The results of this study show that sewage epidemiology provide real-time data for drug abuse.

【关键词】 苯丙胺甲基苯丙胺污水衍生化
【Key words】 AmphetamineMethamphetamineSewageDerivatization
  • 【分类号】X832
  • 【被引频次】2
  • 【下载频次】256
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