Two highly sensitive methods for the determination of genotoxic alkyl methane sulfonates (AMSs) and alkyl paratoluene sulfonates (APTSs) in lamivudine using hyphenated techniques have been presented. AMSs were determi...Two highly sensitive methods for the determination of genotoxic alkyl methane sulfonates (AMSs) and alkyl paratoluene sulfonates (APTSs) in lamivudine using hyphenated techniques have been presented. AMSs were determined by GC-MS method using GSBPINOWAX (30 m 0.25 mm 0.25 mm) column. Temperature program was set by maintaining at 100 1C initially for 3 min, then rised to 220 1C at the rate of 15 1C/min and maintained at 220 1C for 16 min. N,N-dimethyl formamide was used as diluent. APTSs were determined by LC-MS using Zorbax, Rx C8, 250 mm 4.6 mm, 5 mm column as stationary phase. 0.01 M ammonium acetate is used as buffer. The mixture of buffer and methanol in 75:25 (v/v) ratio was used as mobile phase A and mixture of buffer and methanol in 5:95 (v/v) ratio was used as mobile phase B. The gradient program (T/%B) was set as 0/28, 16/50, 17/100, 23/100, 27/28 and 40/28. Both the methods were validated as per International Conference on Harmonization guidelines. Limit of quantitation was found 1.5 mg/mL for AMSs and was in the range of 1.0-1.5 mg/mL for APTSs.展开更多
Introduction Geological resource survey demands for determining various constituents including major, minor, micro, trace and ultra-trace levels of elements for preparing the map of resource distribution of our count...Introduction Geological resource survey demands for determining various constituents including major, minor, micro, trace and ultra-trace levels of elements for preparing the map of resource distribution of our country. As a powerful and popularly used technique for multi-element analysis, inductively coupled plasma（ICP） atomic emission spectrometry （AES） has been applied to this field for a period of time. However, ICP spectrometric determination of those micro, trace and ultratrace elements needs enrichment procedures for improving the detection limit, which is unacceptable in case a great mass of samples should be analyzed as that in the task of geological resource survey. On the other hand, although ICP mass spectrometry （MS） is considered the most powerful method for trace elements determination, it is difficult for ICP-MS to be used to determine the trace and major analytes simultaneously in a spectrum.展开更多
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
文摘Two highly sensitive methods for the determination of genotoxic alkyl methane sulfonates (AMSs) and alkyl paratoluene sulfonates (APTSs) in lamivudine using hyphenated techniques have been presented. AMSs were determined by GC-MS method using GSBPINOWAX (30 m 0.25 mm 0.25 mm) column. Temperature program was set by maintaining at 100 1C initially for 3 min, then rised to 220 1C at the rate of 15 1C/min and maintained at 220 1C for 16 min. N,N-dimethyl formamide was used as diluent. APTSs were determined by LC-MS using Zorbax, Rx C8, 250 mm 4.6 mm, 5 mm column as stationary phase. 0.01 M ammonium acetate is used as buffer. The mixture of buffer and methanol in 75:25 (v/v) ratio was used as mobile phase A and mixture of buffer and methanol in 5:95 (v/v) ratio was used as mobile phase B. The gradient program (T/%B) was set as 0/28, 16/50, 17/100, 23/100, 27/28 and 40/28. Both the methods were validated as per International Conference on Harmonization guidelines. Limit of quantitation was found 1.5 mg/mL for AMSs and was in the range of 1.0-1.5 mg/mL for APTSs.
文摘Introduction Geological resource survey demands for determining various constituents including major, minor, micro, trace and ultra-trace levels of elements for preparing the map of resource distribution of our country. As a powerful and popularly used technique for multi-element analysis, inductively coupled plasma（ICP） atomic emission spectrometry （AES） has been applied to this field for a period of time. However, ICP spectrometric determination of those micro, trace and ultratrace elements needs enrichment procedures for improving the detection limit, which is unacceptable in case a great mass of samples should be analyzed as that in the task of geological resource survey. On the other hand, although ICP mass spectrometry （MS） is considered the most powerful method for trace elements determination, it is difficult for ICP-MS to be used to determine the trace and major analytes simultaneously in a spectrum.
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.
