ABSTRACT
Liquid chromatography tandem mass chromatography (LC-MS/MS) is an important hyphenated technique for quantitative analysis of drugs in biological fluids. Because of high sensitivity and selectivity, LC-MS/MS has been used for pharmacokinetic studies, metabolites identification in the plasma and urine. This manuscript gives comprehensive analytical review, focusing on chromatographic separation approaches (column packing materials, column length and mobile phase) as well as different acquisition modes (SIM, MRM) for quantitative analysis of glucocorticoids and stimulants. This review is not meant to be exhaustive but rather to provide a general overview for detection and confirmation of target drugs using LC-MS/MS and thus useful in the doping analysis, toxicological studies as well as in pharmaceutical analysis.
ABSTRACT
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 μm) column.Temperature program was set by maintaining at 100 ℃ initially for 3 min,then rised to 220 ℃ at the rate of 15 ℃/min and maintained at 220 ℃ 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 μm 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 μg/mL for AMSs and was in the range of 1.0-1.5 μg/mL for APTSs.