科研之友
微信
新浪微博
Facebook
分享链接
摘要
A fast and simple sample cleanup approach for levocetirizine in human was developed using protein precipitation coupled with LC-MS-MS. Samples were treated with 6% trichloroacetic acid in water prior to LC-MS-MS analysis. Chromatographic separation was performed on a reverse phase column with an isocratic mobile phase of acetonitrile and 10 mM ammonium formate pH 3.5 (80: 20, v/v) at a flow rate of 1.0 mL/min. The run time was 3.5 min. Mass parameters were optimized to monitor transitions at m/z [M+H](+) 389.0 -> 201.0 for levocetirizine and m/z [M+H](+) 375.3 -> 201.0 for hydroxyzine as internal standard. The lower limit of quantification and the dynamic range were 1.00 and 1.00-500 ng/mL, respectively. Linearity was good for intraday and interday validations (r(2) >= 0.995). The mean recoveries were 59 and 69% for levocetirizine and hydroxyzine, respectively. Matrix effect was acceptable with %CV < 15. Hemolytic effect was negligible. Levocetirizine was stable in human plasma for 27 h at room temperature (25 degrees C), for 16 weeks frozen at -70 degrees C, 4 weeks frozen at -20 degrees C, for 24 h in an autosampler at 15 degrees C and for three freeze/thaw cycles. The validated method was applied in a pharmacokinetic study to determine the concentration of levocetirizine in plasma samples. The study provides a fast and simple bioanalytical method for routine analysis and may be particularly useful for bioequivalence studies.
- 出版日期2015-12
