Problems of Forensic Sciences 2006 Vol. 66 (LXVI) 212-219
ANALYSIS OF ATROPINE AND SCOPOLAMINE IN BODY FLUIDS
Agnieszka SKULSKA, Maria KAŁA
Institute of Forensic Research, Krakow, Poland
Streszczenie
Methods for determination of atropine (AT) and scopolamine (SK) in biological material (whole blood and urine) using the liquid chromatography atmospheric pressure chemical ionisation mass spectrometry technique (LC-MS/APCI) were developed. Separation of analytes was performed using a LiChroCART LiChrospher 60 RP-select B column in gradient conditions. The mobile phase consisted of 0.1% (v/v) formic acid in water and in acetonitrile. Target analytes were isolated from biological matrices using the liquid-liquid extraction technique. The validation data of the methods were characterised by: limit of detection (LOD, S/N = 3) and limit of quantification (LOQ, S/N = 10) – 0.2 and 0.6 ng ml–1 for SK, and 0.3 and 0.9 ng ml–1 for AT, both in blood, whereas 1.8 and 2.1 ng ml–1 for SK, and 0.6 and 0.9 ng ml–1 for AT in urine. Calibration curves showed linearity in concentration ranges from LOQ to 25 ng ml-1 in blood and from LOQ to 50 ng ml–1 in urine. Determination coefficients (R2) of linear regression equation were higher than 0.98. Extraction recoveries were determined at analytes and internal standard (IS) concentration of 5 ng ml–1 for blood, and at analytes and IS concentrations of 20 and 5 ng ml–1, respectively for urine. Extraction recovery ranged from 80 (AT) to 85% (SK) for blood and 63–72% for urine.
Słowa kluczowe
Atropine; Scopolamine; LC-MS/APCI methods.