UPLC-MS/MS Determination of Phentolamine in Human Plasma and its Application to a Pharmacokinetic Study

X. Kan; S.-l. Zheng; C.-y. Zhou

doi:10.1055/s-0033-1364002

Drug Research, Inhaltsverzeichnis

Drug Res (Stuttg) 2014; 64(11): 607-612
DOI: 10.1055/s-0033-1364002

Original Article

UPLC-MS/MS Determination of Phentolamine in Human Plasma and its Application to a Pharmacokinetic Study

X. Kan

¹Wenzhou People’s Hospital, Wenzhou, China

⁴Yueqing Third People’s Hospital, Wenzhou, China

,

S.-l. Zheng

²The Second Affiliated Hospital of Wenzhou Medical University, Wenzhou, China

,

C.-y. Zhou

³The Third Affiliated Hospital of Wenzhou Medical University, Wenzhou, China

› Institutsangaben

Abstract

A sensitive and rapid ultra performance liquid chromatography tandem mass spectrometry (UPLC-MS/MS) method was developed to determine phentolamine in human plasma. Sample preparation was accomplished through a simple liquid-liquid extraction with ethyl acetate. Chromatographic separation was carried out on an Acquity UPLC BEH C18 column using an isocratic mobile phase system composed of acetonitrile and 1% formic acid in water (33:67, v/v) at a flow rate of 0.45 mL/min. Mass spectrometric analysis was performed using a QTrap5500 mass spectrometer coupled with an electro-spray ionization (ESI) source in the positive ion mode. The MRM transitions of m/z 282.1 → 212.0 and m/z 237.1 → 194.2 were used to quantify for phentolamine and carbamazepine (internal standard, IS), respectively. The linearity of this method was found to be within the concentration range of 0.5–100.0 ng/mL with a lower limit of quantification of 0.5 ng/mL. Only 1.0 min was needed for an analytical run. This fully validated method was successfully applied to the pharmacokinetic study after oral administration of 60 mg phentolamine to 20 Chinese healthy male volunteers.

Key words

phentolamine - UPLC-MS/MS - human plasma - pharmacokinetic

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