GC-MS法分析检验麻黄碱

发布时间：2018-01-04 04:01

本文关键词：GC-MS法分析检验麻黄碱　出处：《甘肃政法学院》2015年硕士论文　论文类型：学位论文

【摘要】：麻黄碱(ephedrine),(1R,2S)-2-甲氨基-苯丙烷-1-醇,一种生物碱,存在于植物麻黄中。麻黄碱可用于治疗过敏性疾病,如支气管哮喘、百日咳、枯草热等,同时,麻黄碱对中枢神经系统有兴奋作用,与苯丙胺类毒品的药理、毒理作用较为相似。麻黄碱不仅是一种兴奋剂,而且还是冰毒的合成原料之一。因此,国内外出台各项规章制度对麻黄碱及含有麻黄碱的药品进行严格管制,如:国际奥委会医学委员会禁止运动员在比赛期间使用含有麻黄碱及其盐类的药品;2005年我国颁布《易制毒化学品管理条例》中将麻黄碱及其盐类规定为国家管制类药品;2011年,在我国修订的《危险化学品安全管理条例》中,麻黄碱被列为公安部门管制物质;2012年,国家食品药品监督管理局限制麻黄碱在最小包装规格中的含量,并指出含麻黄碱类复方制剂仿制药原则上不再被批准注册,同时,应当实名制购买含麻黄碱类复方制剂药品。目前,大部分研究集中在药物中麻黄碱含量的检测,而对于复杂生物检材中麻黄碱的检测方法报道相对较少,因此,本文采用GC-MS法对复杂生物检材中麻黄碱含量的检测进行了研究。本文分别考察了内标、衍生化试剂、衍生化方式、衍生化试剂用量、衍生化时间、色谱柱、升温程序以及质谱条件等方面对麻黄碱检测的影响。同时建立了小鼠血液、肝脏等生物检材中GC-MS测定麻黄碱的方法。实验结果表明,利用GC-MS检测麻黄碱的最佳条件为:气相色谱条件:Elite-35MS石英毛细管柱(30m×0.25mm,0.25μm),进样口温度为270℃,氦气(99.999%),流速1.0m L/min恒流模式,程序升温:80℃→12℃/min→220℃(5min)→12℃/min→280℃(5min),1μL不分流进样。质谱条件:EI源70e V,质量范围:40~500amu,离子源温度:250℃,传输线温度:250℃,载气:高纯氦气(99.999%),流速1.0m L/min恒流模式。测定血液中麻黄碱的线性回归方程Y=1.67326X+35.6341,线性范围50~500ng/m L,检测限11ng/m L,回收率为89.47~104.43%;测定肝脏中麻黄碱的线性回归方程Y=1.67326X+35.6341,线性范围50~500ng/m L,检测限17ng/m L,回收率为97.89~102.13%;测定毛发中麻黄碱的线性回归方程Y=2.78934X+58.3878,线性范围50~500ng/m L,检测限39ng/m L,回收率为84.70%~93.25%。利用建立的GC-MS检测方法测定了麻黄碱中毒小鼠的血液、肝脏等样品,结果在血液、肝脏中均检测到麻黄碱,说明该方法可用于测定复杂生物检材中的痕量麻黄碱,效果较好。
[Abstract]:Ephedrine (ephedrine), (1R, 2S) -2- dimethylamino - benzene propane -1- alcohol, an alkaloid present in plant ephedra. Ephedrine can be used for the treatment of allergic diseases, such as asthma, hay fever, whooping cough, etc., at the same time, there is excitement with ephedrine on the central nervous system, pharmacology and amphetamines the toxicological effects of ephedrine is similar. Not only is a stimulant, one of the synthetic materials and methamphetamine. Therefore, the introduction of domestic and foreign regulations on drugs containing ephedrine and ephedrine are strictly controlled, such as: International Olympic Committee Medical Commission banned athletes use drugs containing ephedrine and its salts during the game; in 2005 China promulgated < the easy administration of precursor chemicals, ephedrine and its salts, > provisions for the control of the state drug; in 2011, in the "Regulations of safety management of hazardous chemicals in China revised >, ephedra Alkali was classified as a public security department in 2012, the content of controlled substances; minimum packaging specifications in the State Food and Drug Administration restrictions ephedrine, and pointed out that the compound preparations containing ephedrine generics in principle no longer approved registration shall, at the same time, the real name system purchase contain ephedrine kind of compound preparation drugs. At present, most of the studies focus detection of ephedrine in medicine, the reported detection method of ephedrine complex in biological samples is relatively small, therefore, this paper uses the GC-MS method to detect the content of ephedrine in complex biological samples were studied. The paper studied the internal standard, derivatization reagent, the derivatization reagent dosage, derivatization, derivatization time that column, effects of heating conditions on mass spectrometry procedures and ephedrine detection. While establishing mouse blood, determination of ephedrine GC-MS liver in biological samples Method. The experimental results show that the optimum conditions for the detection of ephedrine GC-MS: gas chromatographic conditions: Elite-35MS quartz capillary column (30M * 0.25mm, 0.25 m), the inlet temperature is 270 DEG C, helium (99.999%), the flow rate of 1.0m L/min in constant current mode, programmed temperature: 80 degrees, 12 degrees, /min 220 C (5min), 12 /min to 280 DEG C (5min), 1 L splitless. Mass spectrometry conditions: EI source 70E V, quality range: 40~500amu, ion source temperature: 250 degrees centigrade, transmission line temperature: 250 C, carrier gas: pure helium (99.999%), the flow rate of 1.0m L/min the constant current mode. The determination of ephedrine in blood of linear regression equation is Y=1.67326X+35.6341, linear range of 50~500ng/m L, the detection limit of 11ng/m L, the recovery rate is 89.47~104.43%; Determination of ephedrine in liver of linear regression equation is Y=1.67326X+35.6341, linear range of 50~500ng/m L, the detection limit of 17ng/m L, the recovery rate is 97.89~102.13%; Determination of ephedrine in the hair line The regression equation of Y=2.78934X+58.3878, the linear range of 50~500ng/m L, the detection limit of 39ng/m L, the recovery rate was 84.70%~93.25%. ephedrine poisoning of mice was measured by blood GC-MS detection method established, liver samples, results in blood and liver were detected in ephedrine, show that the proposed method can be used for the determination of trace ephedrine, complex in biological samples the effect is good.

【学位授予单位】：甘肃政法学院
【学位级别】：硕士
【学位授予年份】：2015
【分类号】：D918.93

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