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

Autor*innen

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

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

Volltext

Referenzen

References
1 Moore PA, Hersh EV, Papas AS et al. Pharmacokinetics of lidocaine with epinephrine following local anesthesia reversal with phentolamine mesylate. Anesth Prog 2008; 55: 40-48
2 Hersh EV, Moore PA, Papas AS et al. Reversal of soft-tissue local anesthesia with phentolamine mesylate in adolescents and adults. J Am Dent Assoc 2008; 139: 1080-1093
3 Elmore S, Nusstein J, Drum M et al. Reversal of Pulpal and Soft Tissue Anesthesia by Using Phentolamine: A Prospective Randomized, Single-blind Study. J Endod 2013; 39: 429-434
4 Tavares M, Goodson JM, Studen-Pavlovich D et al. Reversal of soft-tissue local anesthesia with phentolamine mesylate in pediatric patients. J Am Dent Assoc 2008; 139: 1095-1104
5 Moradkhan R, Spitnale B, McQuillan P et al. Hypoxia-induced vasodilation and effects of regional phentolamine in awake patients with sleep apnea. J Appl Physiol 2010; 108: 1234-1240
6 Laviola M, McGavin SK, Freer GA et al. Randomized study of phentolamine mesylate for reversal of local anesthesia. J Dent Res 2008; 87: 635-639
7 Froum SJ, Froum SH, Malamed SF. The use of phentolamine mesylate to evaluate mandibular nerve damage following implant placement. Compend Contin Educ Dent 2010; 31 (520) 522-528
8 Fowler S, Nusstein J, Drum M et al. Reversal of soft-tissue anesthesia in asymptomatic endodontic patients: a preliminary, prospective, randomized, single-blind study. J Endod 2011; 37: 1353-1358
9 Webster GK, Lemmer RR, Greenwald S. Rapid analysis of phentolamine by high-performance liquid chromatography. J Chromatogr Sci 2003; 41: 57-62
10 Kerger BD, James RC, Roberts SM. An assay for phentolamine using high performance liquid chromatography with electrochemical detection. Anal Biochem 1988; 170: 145-151
11 Godbillon J, Carnis G. Determination of the major metabolite of phentolamine in human plasma and urine by high-performance liquid chromatography. J Chromatogr 1981; 222: 461-466
12 de Bros F, Wolshin EM. Determination of phentolamine in blood and urine by high performance liquid chromatography. Anal Chem 1978; 50: 521-525
13 Wu L, Liu J, Zhang Y et al. Development of a HPLC/MS/MS method for simultaneous determination of tinidazole, dyclonine and chlorhexidine in rat plasma and its application in the pharmacokinetic research of a film-forming solution. J Pharm Biomed Anal 2012; 62: 224-227
14 Wu JT. The development of a staggered parallel separation liquid chromatography/tandem mass spectrometry system with on-line extraction for high-throughout screening of drug candidates in biological fluids. Rapid Commun Mass Spectrom 2001; 15: 73-81
15 Silva LF, Moraes MO, Santana GS et al. Phentolamine bioequivalence study. Int J Clin Pharmacol Ther 2004; 42: 43-49
16 Mikami E, Ohno T, Matsumoto H. Simultaneous identification/determination system for phentolamine and sildenafil as adulterants in soft drinks advertising roborant nutrition. Forensic Sci Int 2002; 130: 140-146
17 Xing LL, Tang YH, Wang ZC et al. Sensitive chemiluminescence determination of phentolamine mesylate and phenoxybenzamine hydrochloride based on K3Fe(CN)(6)-H2O2-fluorescein. Journal of Luminescence 2013; 137: 162-167
18 Huang Y, Liu W. Flow-injection chemiluminescence determination of phentolamine based on its enhancing effect on the luminol-potassium ferricyanide system. J Pharm Biomed Anal 2005; 38: 537-542
19 de Villiers A, Lestremau F, Szucs R et al. Evaluation of ultra performance liquid chromatography. Part I. Possibilities and limitations. J Chromatogr A 2006; 1127: 60-69
20 Jamalapuram S, Vuppala PK, Abdelazeem AH et al. Ultra-performance liquid chromatography tandem mass spectrometry method for the determination of AZ66, a sigma receptor ligand, in rat plasma and its application to in vivo pharmacokinetics. Biomed Chromatogr 2013; 27: 1034-1040