PMID- 12052724
OWN - NLM
STAT- MEDLINE
DCOM- 20020822
LR  - 20190922
IS  - 1570-0232 (Print)
IS  - 1570-0232 (Linking)
VI  - 774
IP  - 1
DP  - 2002 Jul 5
TI  - Determination of ketoconazole in human plasma by high-performance liquid 
      chromatography-tandem mass spectrometry.
PG  - 67-78
AB  - A simple, rapid and specific high-performance liquid chromatography coupled with 
      tandem mass spectrometry (LC-MS-MS) has been developed and validated for the 
      determination of ketoconazole in human plasma. The method used diethyl ether to 
      extract the ketoconazole and the internal standard (I.S.) R51012 from alkalinized 
      plasma sample. The LC separation was on a C(18) column (50 x 3 mm, 5 microm) 
      using acetonitrile-water-formic acid (75:25:1, v/v/v) mobile phase. The retention 
      times were approximately 1.8 min for both ketoconazole and the I.S. The MS-MS 
      detection was by monitoring 531.2-->82.1 (m/z) for ketoconazole, and 
      733.5-->460.2 (m/z) for the I.S. The dynamic range was from 20.0 to 10000 ng/ml 
      based on 0.1 ml plasma, with linear correlation coefficient of > or =0.9985. The 
      run time was 2.5 min/injection. The recoveries of ketoconazole and the I.S. were 
      102 and 106%, respectively. The precision and accuracy of the control samples 
      were with the relative standard deviations (RSDs) of < or =4.4% (n=6) and the 
      relative errors (REs) from -0.6 to 1.4% for intra-day assay, and < or =8.6% RSD 
      (n=18) and -1.4 to 0.9% RE for inter-day assay. The partial volume tests 
      demonstrated good dilution integrity. Three freeze-thaw cycles, keeping plasma 
      samples at ambient for 24 h, storing extracted samples at ambient for 24 h, and 
      storing frozen plasma samples at approximately -20 degrees C for up to 2 months 
      did not show substantial effects.
FAU - Chen, Yu-Luan
AU  - Chen YL
AD  - Department of Bioanalytical Chemistry, Covance Laboratories Inc., 3301 Kinsman 
      Boulevard, Madison, WI 53704, USA. yuluan.chen@covance.com
FAU - Felder, L
AU  - Felder L
FAU - Jiang, Xiangyu
AU  - Jiang X
FAU - Naidong, Weng
AU  - Naidong W
LA  - eng
PT  - Journal Article
PL  - Netherlands
TA  - J Chromatogr B Analyt Technol Biomed Life Sci
JT  - Journal of chromatography. B, Analytical technologies in the biomedical and life 
      sciences
JID - 101139554
RN  - 0 (Antifungal Agents)
RN  - R9400W927I (Ketoconazole)
SB  - IM
MH  - Antifungal Agents/*blood
MH  - Chromatography, High Pressure Liquid/*methods
MH  - Humans
MH  - Ketoconazole/*blood
MH  - Mass Spectrometry/*methods
MH  - Reference Standards
MH  - Reproducibility of Results
MH  - Sensitivity and Specificity
EDAT- 2002/06/08 10:00
MHDA- 2002/08/23 10:01
CRDT- 2002/06/08 10:00
PHST- 2002/06/08 10:00 [pubmed]
PHST- 2002/08/23 10:01 [medline]
PHST- 2002/06/08 10:00 [entrez]
AID - S157002320200209X [pii]
AID - 10.1016/s1570-0232(02)00209-x [doi]
PST - ppublish
SO  - J Chromatogr B Analyt Technol Biomed Life Sci. 2002 Jul 5;774(1):67-78. doi: 
      10.1016/s1570-0232(02)00209-x.