Quantitative determination of piritramide in human serum applying liquid chromatography-two-stage mass spectrometry.
A method for the determination of the synthetic narcotic analgesic piritramide in human serum utilizing high-performance liquid chromatography with atmospheric pressure chemical ionization two-stage mass spectrometry (HPLC-APCI-MS-MS) is presented. Pipamperone is used as the internal standard. Serum samples are prepared by liquid-liquid extraction under basic conditions with 1-chlorobutane. The chromatographic separation is achieved on an RP-18 stationary phase applying gradient elution with methanol-0.02% trifluoroacetic acid in water. Detection is carried out in the MS-MS single reaction monitoring mode of the ion-trap mass spectrometer. The limit of detection is 0.3 ng/ml and the calibration covers the range of 1-80 ng/ml. The intra-day RSDs are 6.1 to 7.3% over the calibration range, whereas the inter-day RSDs are 9.6 to 12.8%.
Martens-Lobenhoffer
J
J
Institute of Clinical Pharmacology, Otto-von-Guericke-University Magdeburg, Leipziger Strasse 44, D-39120, Magdeburg, Germany. jens.martens-lobenhoffer@medizin.uni-magdeburg.de
Römhild
W
W
D000701:Analgesics, Opioid / Q000097:blood*; D002851:Chromatography, High Pressure Liquid / Q000379:methods*; D006801:Humans; D013058:Mass Spectrometry / Q000379:methods*; D010892:Pirinitramide / Q000097:blood*; D012015:Reference Standards; D015203:Reproducibility of Results; D012680:Sensitivity and Specificity
D000701:Analgesics, Opioid; D010892:Pirinitramide