Development and validation of a LC-MS/MS method for the determination of clebopride and its application to a pharmacokinetics study in healthy Chinese volunteers.
A sensitive and specific liquid chromatography-electrospray ionization-mass spectrometry (LC-ESI-MS/MS) method has been developed and validated for the identification and quantification of clebopride in human plasma using itopride as an internal standard. The method involves a simple liquid-liquid extraction. The analytes were separated by isocratic gradient elution on a CAPCELL MG-III C(18) (5 microm, 150 mm x 2.1 mm i.d.) column and analyzed in multiple reaction monitoring (MRM) mode with positive electrospray ionization (ESI) interface using the respective [M+H](+) ions, m/z 373.9-->m/z184.0 for clebopride, m/z 359.9-->m/z71.5 for itopride. The method was validated over the concentration range of 69.530-4450.0 pg/ml for clebopride. Within- and between-batch precision (RSD%) was all within 6.83% and accuracy ranged from -8.16 to 1.88%. The LLOQ was 69.530 pg/ml. The extraction recovery was on an average 77% for clebopride. The validated method was used to study the pharmacokinetics profile of clebopride in human plasma after oral administration of clebopride.
Tan
Zhirong
Z
Pharmacogenetics Research Institute, Institute of Clinical Pharmacology, Central South University, Xiangya Road 110, Changsha, Hunan 410078, PR China.
Ouyang
Dongsheng
D
Chen
Yao
Y
Zhou
Gan
G
Cao
Shan
S
Wang
Yicheng
Y
Peng
Xiujuan
X
Zhou
Honghao
H
D000284:Administration, Oral; D000932:Antiemetics / Q000008:administration & dosage / Q000097:blood* / Q000737:chemistry / Q000493:pharmacokinetics*; D044466:Asian People; D001549:Benzamides / Q000008:administration & dosage / Q000097:blood* / Q000737:chemistry / Q000493:pharmacokinetics*; D001593:Benzyl Compounds / Q000097:blood / Q000737:chemistry; D002853:Chromatography, Liquid / Q000379:methods*; D004355:Drug Stability; D006262:Health; D006801:Humans; D057230:Limit of Detection; D008297:Male; D011786:Quality Control; D012015:Reference Standards; D015203:Reproducibility of Results; D013997:Time Factors
D000932:Antiemetics; D001549:Benzamides; D001593:Benzyl Compounds; C102254:itopride; C014417:clebopride