Ma Jianshe, Dong Jianyong, Lin Guanyang, Yue Lei, Xiang Zheng, Xu Renai, Hu Lufeng, Wang Xianqin
Function Experiment Teaching Center of Wenzhou Medical College, Wenzhou 325035, China.
Biomed Chromatogr. 2012 May;26(5):655-9. doi: 10.1002/bmc.1711. Epub 2011 Sep 19.
A sensitive and selective liquid chromatography mass spectrometry method for determination of curdione in rabbit plasma was developed. After addition of tramadol as internal standard (IS), protein precipitation by acetonitrile was used for sample preparation. Chromatographic separation was achieved on a Zorbax SB-C₁₈ (2.1 × 50 mm, 3.5 µm) column with acetonitrile-0.1% formic acid as mobile phase with gradient elution. An electrospray ionization source was applied and operated in positive-ion mode; selective ion monitoring was used for quantification using target fragment ions m/z 237 for curdione and m/z 264 for the IS. Calibration plots were linear over the range of 20-4000 ng/mL for curdione in plasma. The lower limit of quantification for curdione was 20 ng/mL. Mean recovery of curdione from plasma was in the range 94.3-98.4%. The RSD of intra-day and inter-day precision were both less than 9%. This method is simple and sensitive enough to be used in pharmacokinetic research for the determination of curdione in rabbit plasma.
建立了一种灵敏且选择性好的液相色谱-质谱法用于测定兔血浆中莪术二酮的含量。加入曲马多作为内标后，采用乙腈沉淀蛋白法进行样品制备。在Zorbax SB-C₁₈（2.1×50 mm，3.5 µm）色谱柱上，以乙腈-0.1%甲酸为流动相进行梯度洗脱，实现色谱分离。采用电喷雾电离源，以正离子模式运行；使用选择性离子监测模式，以莪术二酮的目标碎片离子m/z 237和内标的目标碎片离子m/z 264进行定量分析。血浆中莪术二酮在20 - ⁴⁰⁰⁰ ng/mL范围内校准曲线呈线性。莪术二酮的定量下限为20 ng/mL。莪术二酮从血浆中的平均回收率在94.3% - 98.4%范围内。日内和日间精密度的相对标准偏差均小于9%。该方法简单且灵敏，可用于兔血浆中莪术二酮的药代动力学研究。
