Development and validation of 2-deoxy-2-chloro- d -glucose impurity analysis in [18 F]FDG by three potential-time waveforms of high-performance liquid chromatography/pulsed amperometric detection

• Published in: Nuclear medicine and biology Vol. 36; no. 2; pp. 225 - 231
• Main Authors: Farn, Shiou-Shiow, Yeh, Yuen-Han, Lin, Wuu-Jyh, Shen, Lie-Hang
• Format: Journal Article
• Language: English
• Published: United States Elsevier Inc 01.02.2009
• Subjects: [ 18F]FDG, ClDG, HPLC, Pulsed amperometric detection (PAD), Gold working electrode; Chromatography, High Pressure Liquid - methods; Deoxyglucose - analogs & derivatives; Deoxyglucose - analysis; Drug Contamination; Electrochemistry; Fluorodeoxyglucose F18 - analysis; Palladium reference electrode; Radiology; Radiopharmaceuticals - analysis; Reproducibility of Results; Temperature; [ 18F]FDG, ClDG, HPLC, Pulsed amperometric detection (PAD), Gold working electrode; Palladium reference electrode
• ISSN: 0969-8051; 1872-9614
• DOI: 10.1016/j.nucmedbio.2008.11.008

Abstract A suitable three potential-time waveforms for the electrochemical detection of 2-deoxy-2-chloro- d -glucose (ClDG) by gold working electrode and palladium reference electrode have been developed and method validation was performed on Waters 2796 Bioalliance HPLC system coupled with pulsed amperometric detection (HPLC/PAD). FDG and ClDG could be completely separated by 50 mM NaOH mobile phase at a flow rate of 1.0 ml/min; 30°C analytical column temperature; and E1 of 200 mV, T1 of 900 mS; E2 of −770 mV, T2 of 10 mS; E3 of 1400 mV, T3 of 10 mS; acquisition delay (AD) of 300 mS. The validation results were shown as follows: (1) in specificity study, mannose, FDG and ClDG could be completely separated and the retention times of these were 6.2, 11.1 and 13.5 min, respectively, with a total run time of 20 min; (2) the intraday repeatable precision expressed with the CV% in six successive analysis was 0.52% (for FDG) and 0.83% (for ClDG); (3) the interday variability precision expressed with the CV% value of the repeatable precision of 3 days was 0.99%, 0.52% and 0.58% for FDG and 0.71%, 0.83% and 1.24% for ClDG; both the CV% of intraday and interday reproducibilities of FDG and ClDG were better than 1.5%; (4) the accuracy and recovery of FDG and ClDG expressed with the percentage of mean value of three successive analysis were 99.75% (for FDG) and 100.68% (for ClDG) which were all greater than 95%; (5) under optimum conditions, the limit of detection of FDG and ClDG was 0.41 and 0.68 μg/ml, and the limit of quantization of FDG and ClDG was 1.24 and 2.04 μg/ml; (6) the correlation coefficient ( r ) value of linearity is over 0.999 by 5–50 μg/ml ranges of both compounds, respectively; (7) no interference peak effects by composition of mobile phase or increasing/decreasing flow rate or change of temperature was observed.