Rapid Determination of Caffeine in Forensic Aqueous Sample by Dilute and Shoot LC-MS/MS

A liquid chromatography-tandem mass spectrometry (LC-MS/MS) method was developed and validated for the determination of caffeine in forensic aqueous sample. The centrifuged sample ($100{\mu}l$) was diluted 50-fold with distilled water. The diluted sample ($400{\mu}l$) was then diluted further with $200{\mu}l$ of 0.1% formic acid solution and $400{\mu}l$ of acetonitrile containing 500 ng of caffeine-(3-methyl-$^{13}C_3$) prior to LC-MS/MS analysis. The mobile phase was composed of 0.1% formic acid in distilled water (A) and acetonitrile (B). Chromatographic separation was performed by using a Zorbax SB-C18 ($100mm{\times}2.1mm$ i.d., $3.5{\mu}m$) column and caffeine was eluted within 1.1 min. Linear least-squares regression with a 1/x weighting factor was used to generate a calibration curve with the coefficients of determination ($r^2=0.9983$). The lower limit of quantification was $25ng/ml$ for the analyte. The process efficiency was 98.6~100.1%. Intra- and inter-day precisions were not more than 2.1% and 1.7%, while intra- and inter-day accuracies were ranged from -6.8 to 4.5%, respectively. The suitability of the method was examined by analyzing unknown forensic aqueous samples.

시료 희석 직접 주입 LC-MS/MS를 이용한 법화학 수용액 시료 중 카페인 신속 분석