适于常规血药浓度监测的LC／LC-UV卡马西平方法研究

目的建立基于LC／LC-UV系统的卡马西平血药浓度测定的方法，此方法适于长期的治疗药物浓度监测。方法LC1色谱柱为FRO-）（BC18（33mm×4．6mm，5μm，UAC），流动相为水-乙腈（60：40，v／v），流速为1．0mL·min^-1，检测波长为286nm，温度为45℃；LC2系统中色谱柱为UC—XBC18（250mm×4．6mm，5μm，UAC），流动相为0．3％的醋酸铵（用甲酸调pH到6．50）-乙腈（75：35，v／v），流速为1．2mL·min^-1，检测波长为286nm；聚焦溶液为二次蒸馏水，进样聚焦流速为3．5mL·min^-1，目标物从LC1转移到LC2聚焦流速为1．0mL·min^-1，中心切换窗口为1．09～1．60min；定量环为200μL。结果卡马西平在1．10-21．30μg·mL^-1线性关系良好，平均相关系数为0．9994，最低定量浓度为15．0ng·mL^-1。日内、日间RSD均〈10％（n=6）。结论本方法准确性高、精密度好、操作步骤少、耐受性强且易于实现质量控制，适合于长期的卡马西平常规血药浓度监测。

Routine quantitative measurements of carbamazepine in the plasma by LC/LC-UV

Objective To establish a routine analytical method for the determination of earbamazepine by LC/LC-UV , and for the therapeutic drug monitoring of carbamazepine. Methods LC1 system column was FRO-XB C18 （33 min×4.6 mm, 5 μm, UAC）, with mobile phase consisting of water-acetonitrile （60 ： 40, v/v） at the flow rate of 1.0 mL·min^-1. The detection wavelength was 286 nm and column temperature was 45 ℃. LC2 system column was UC-XB C18 （250 min×4.6 mm, 5 μm, UAC）, with mobile phase consisting of 0.3% ammonium acetate （pH 6.50 adjusted by formic acid） - acetonitrile （75 ： 35, v/v） at the flow rate of 1.2 mL·min^-1. The detection wavelength was 286 nm and column temperature was 45 ℃ . The focusing solution was redistilled water and flow rate of injection was 3.5 mL· min^-1. Flow of transferring was 1.0 mL·min^-1 , and the windows of ＂heart cutting＂ was 1.09-1.60 min. The sample loop volume was 200 kcL. Results The linearity range of carbamazepine was 1. 10-21.30μg ·mL^-1 （r=0. 999 4）. The limit of quantification was 15.0 ng·mL^-1. The intra-day and inter-day precision and RSD was 10%（n=6）. Conclusion The method is accurate, fast, simple, and easy to establish quality control, the method is the routine blood drug moniter of earbamazepine.