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KMID : 0370220160600030112
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Yakhak Hoeji
2016 Volume.60 No. 3 p.112 ~ p.117
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Rapid Determination of Caffeine in Forensic Aqueous Sample by Dilute and Shoot LC-MS/MS
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Choi Yun-Jeong
Kim Hee-Seung
In Moon-Kyo
Kim Jin-Young
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Abstract
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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 꺤l) was diluted 50-fold with distilled water. The diluted sample (400 꺤l) was then diluted further with 200 꺤l of 0.1% formic acid solution and 400 꺤l of acetonitrile containing 500 ng of caffeine-(3-methyl-13C3) 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 (100 mm?2.1 mm i.d., 3.5 꺤m) 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 (r2=0.9983). The lower limit of quantification was 25 ng/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.
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KEYWORD
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caffeine, dilute and shoot, HPLC, mass spectrometry, forensic sample
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