title: 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.
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 degrees 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 microg/ml, and the limit of quantization of FDG and ClDG was 1.24 and 2.04 microg/ml; (6) the correlation coefficient (r) value of linearity is over 0.999 by 5-50 microg/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.
authors.affiliation: Isotope Application Division, Institute of Nuclear Energy Research, Taoyuan County, Taiwan (ROC). amanda@iner.gov.tw
authors.forename: Shiou-Shiow
authors.initials: SS
authors.lastname: Farn
authors.forename: Yuen-Han
authors.initials: YH
authors.lastname: Yeh
authors.forename: Wuu-Jyh
authors.initials: WJ
authors.lastname: Lin
authors.forename: Lie-Hang
authors.initials: LH
authors.lastname: Shen
mesh_terms: D002851:Chromatography, High Pressure Liquid / Q000379:methods*; D003847:Deoxyglucose / Q000031:analogs & derivatives* / Q000032:analysis; D004340:Drug Contamination; D004563:Electrochemistry; D019788:Fluorodeoxyglucose F18 / Q000032:analysis*; D019275:Radiopharmaceuticals / Q000032:analysis*; D015203:Reproducibility of Results; D013696:Temperature
chemical_list: D019275:Radiopharmaceuticals; D019788:Fluorodeoxyglucose F18; C078464:2-chloro-2-deoxyglucose; D003847:Deoxyglucose