本文關(guān)鍵詞：GC-MS法分析檢驗麻黃堿　出處：《甘肅政法學(xué)院》2015年碩士論文　論文類型：學(xué)位論文

  更多相關(guān)文章： 麻黃堿 GC-MS 檢測 血液 肝臟

【摘要】：麻黃堿(ephedrine),(1R,2S)-2-甲氨基-苯丙烷-1-醇,一種生物堿,存在于植物麻黃中。麻黃堿可用于治療過敏性疾病,如支氣管哮喘、百日咳、枯草熱等,同時,麻黃堿對中樞神經(jīng)系統(tǒng)有興奮作用,與苯丙胺類毒品的藥理、毒理作用較為相似。麻黃堿不僅是一種興奮劑,而且還是冰毒的合成原料之一。因此,國內(nèi)外出臺各項規(guī)章制度對麻黃堿及含有麻黃堿的藥品進行嚴格管制,如:國際奧委會醫(yī)學(xué)委員會禁止運動員在比賽期間使用含有麻黃堿及其鹽類的藥品;2005年我國頒布《易制毒化學(xué)品管理條例》中將麻黃堿及其鹽類規(guī)定為國家管制類藥品;2011年,在我國修訂的《危險化學(xué)品安全管理條例》中,麻黃堿被列為公安部門管制物質(zhì);2012年,國家食品藥品監(jiān)督管理局限制麻黃堿在最小包裝規(guī)格中的含量,并指出含麻黃堿類復(fù)方制劑仿制藥原則上不再被批準(zhǔn)注冊,同時,應(yīng)當(dāng)實名制購買含麻黃堿類復(fù)方制劑藥品。目前,大部分研究集中在藥物中麻黃堿含量的檢測,而對于復(fù)雜生物檢材中麻黃堿的檢測方法報道相對較少,因此,本文采用GC-MS法對復(fù)雜生物檢材中麻黃堿含量的檢測進行了研究。本文分別考察了內(nèi)標(biāo)、衍生化試劑、衍生化方式、衍生化試劑用量、衍生化時間、色譜柱、升溫程序以及質(zhì)譜條件等方面對麻黃堿檢測的影響。同時建立了小鼠血液、肝臟等生物檢材中GC-MS測定麻黃堿的方法。實驗結(jié)果表明,利用GC-MS檢測麻黃堿的最佳條件為:氣相色譜條件:Elite-35MS石英毛細管柱(30m×0.25mm,0.25μm),進樣口溫度為270℃,氦氣(99.999%),流速1.0m L/min恒流模式,程序升溫:80℃→12℃/min→220℃(5min)→12℃/min→280℃(5min),1μL不分流進樣。質(zhì)譜條件:EI源70e V,質(zhì)量范圍:40~500amu,離子源溫度:250℃,傳輸線溫度:250℃,載氣:高純氦氣(99.999%),流速1.0m L/min恒流模式。測定血液中麻黃堿的線性回歸方程Y=1.67326X+35.6341,線性范圍50~500ng/m L,檢測限11ng/m L,回收率為89.47~104.43%;測定肝臟中麻黃堿的線性回歸方程Y=1.67326X+35.6341,線性范圍50~500ng/m L,檢測限17ng/m L,回收率為97.89~102.13%;測定毛發(fā)中麻黃堿的線性回歸方程Y=2.78934X+58.3878,線性范圍50~500ng/m L,檢測限39ng/m L,回收率為84.70%~93.25%。利用建立的GC-MS檢測方法測定了麻黃堿中毒小鼠的血液、肝臟等樣品,結(jié)果在血液、肝臟中均檢測到麻黃堿,說明該方法可用于測定復(fù)雜生物檢材中的痕量麻黃堿,效果較好。
[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.

【學(xué)位授予單位】：甘肅政法學(xué)院
【學(xué)位級別】：碩士
【學(xué)位授予年份】：2015
【分類號】：D918.93

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