Drugs are traditionally been identified on basis of chromatographic-spectroscopic hyphenated techniques in instrumental analysis. Gas chromatography (GC) and Liquid chromatography (LC) hyphenated with mass spectroscop...Drugs are traditionally been identified on basis of chromatographic-spectroscopic hyphenated techniques in instrumental analysis. Gas chromatography (GC) and Liquid chromatography (LC) hyphenated with mass spectroscopy (MS) i.e. GC-MS and LC-MS give reliable and confirmatory results in drugs identification. In the present work the novel hyphenated technique High Performance Thin Layer Chromatography-Mass Spectroscopy (HPTLC-MS) has been used. This technique provides efficient, quick and simple method for identification and separation of Narcotic drugs and psychotropic substances. The drugs under study are Papaverine, Methadone, Cocaine, Ketamine, Caffeine, Codeine, Diazepam, Thebaine, Heroin, Methamphetamine, Carbamazepine, Morphine, Narcotine and Ephedrine. The present study comprising of sixteen drugs has been carried out on CAMAG HPTLC instrument with automatic sampling. Thin layer chromatography (TLC) plates were developed in various solvent systems, scanned under TLC scanner and the results in terms of Retention Factor (Rf value) and UV spectrum (λmax) are presented in the manuscript. Using hyphenated technique of HPTLC-MS (MS 2020 SHIMADZU) spots of these drugs from TLC plate was lifted with CAMAG TLC-MS interface and confirmed by the mass spectrum of the individual drugs by their m/z values thus delivering fast and accurate confirmatory result on the TLC plate.展开更多
采用液相色谱在线联用电化学反应装置(ECI)对药物氧化加速降解试验进行改进。以叔丁基对苯二酚为模型药物,对高压六通切换阀的切换时间、库仑电化学检测器的操作电压、输液泵流速进行筛选,并通过HPLC-UV检测原型和氧化产物的含量变化,...采用液相色谱在线联用电化学反应装置(ECI)对药物氧化加速降解试验进行改进。以叔丁基对苯二酚为模型药物,对高压六通切换阀的切换时间、库仑电化学检测器的操作电压、输液泵流速进行筛选,并通过HPLC-UV检测原型和氧化产物的含量变化,确定最优的氧化破坏实验条件,最后采用高效液相色谱-二级阵列管检测法对氧化产物进行初步鉴定。结果表明,采用ECI系统进行药物氧化降解试验的最优条件为:六通阀切换时间为30 s,库仑检测器氧化电压为150 m V,输液泵流速为0.2 m L/min。氧化产物经初步鉴定为叔丁基苯醌(TQ)。此装置及其方法可有效缩短时间和简化步骤,实现氧化加速降解试验从样品处理到分离检测的自动化和在线化。展开更多
文摘Drugs are traditionally been identified on basis of chromatographic-spectroscopic hyphenated techniques in instrumental analysis. Gas chromatography (GC) and Liquid chromatography (LC) hyphenated with mass spectroscopy (MS) i.e. GC-MS and LC-MS give reliable and confirmatory results in drugs identification. In the present work the novel hyphenated technique High Performance Thin Layer Chromatography-Mass Spectroscopy (HPTLC-MS) has been used. This technique provides efficient, quick and simple method for identification and separation of Narcotic drugs and psychotropic substances. The drugs under study are Papaverine, Methadone, Cocaine, Ketamine, Caffeine, Codeine, Diazepam, Thebaine, Heroin, Methamphetamine, Carbamazepine, Morphine, Narcotine and Ephedrine. The present study comprising of sixteen drugs has been carried out on CAMAG HPTLC instrument with automatic sampling. Thin layer chromatography (TLC) plates were developed in various solvent systems, scanned under TLC scanner and the results in terms of Retention Factor (Rf value) and UV spectrum (λmax) are presented in the manuscript. Using hyphenated technique of HPTLC-MS (MS 2020 SHIMADZU) spots of these drugs from TLC plate was lifted with CAMAG TLC-MS interface and confirmed by the mass spectrum of the individual drugs by their m/z values thus delivering fast and accurate confirmatory result on the TLC plate.
文摘采用液相色谱在线联用电化学反应装置(ECI)对药物氧化加速降解试验进行改进。以叔丁基对苯二酚为模型药物,对高压六通切换阀的切换时间、库仑电化学检测器的操作电压、输液泵流速进行筛选,并通过HPLC-UV检测原型和氧化产物的含量变化,确定最优的氧化破坏实验条件,最后采用高效液相色谱-二级阵列管检测法对氧化产物进行初步鉴定。结果表明,采用ECI系统进行药物氧化降解试验的最优条件为:六通阀切换时间为30 s,库仑检测器氧化电压为150 m V,输液泵流速为0.2 m L/min。氧化产物经初步鉴定为叔丁基苯醌(TQ)。此装置及其方法可有效缩短时间和简化步骤,实现氧化加速降解试验从样品处理到分离检测的自动化和在线化。
