Hua Wenyan, Ding Li, Chen Yan, Gong Bin, He Jianchang, Xu Guili
Department of Pharmaceutical Analysis, China Pharmaceutical University, 24 Tongjiaxiang, Nanjing 210009, China.
J Pharm Biomed Anal. 2007 Aug 15;44(4):931-7. doi: 10.1016/j.jpba.2007.03.022. Epub 2007 Mar 30.
A liquid chromatography-electrospray ionization-mass spectrometry (LC-ESI-MS) method for the determination of berberine in human plasma using chlorobenzylidine as the internal standard (IS) has been developed and validated. The plasma samples were prepared by LLE and the analytes were chromatographically separated on a Hanbon Lichrospher 5-C18 HPLC column under gradient elution with a mobile phase consisted of acetonitrile and 10mm ammonium acetate buffer containing 0.1% formic acid. Berberine was determined with electrospray ionisation-mass spectrometry (ESI-MS). LC-ESI-MS was performed in the selected-ion monitoring (SIM) mode using target ions at M(+)m/z 336.1 for berberine and M(+)m/z 464.1 for the IS. Calibration curve was linear over the range of 0.020-3.0 ng/ml. The lower limit of quantification (LLOQ) was 0.020 ng/ml. The intra- and inter-run variability values were less than 6.7 and 7.7%, respectively. The method has been successfully applied to determine the plasma concentration of berberine in healthy Chinese volunteers.
已建立并验证了一种以氯苄啶为内标（IS）测定人血浆中黄连素的液相色谱-电喷雾电离-质谱（LC-ESI-MS）方法。血浆样品采用液液萃取（LLE）制备，分析物在汉邦Lichrospher 5-C18高效液相色谱柱上进行色谱分离，流动相为乙腈和含0.1%甲酸的10 mM醋酸铵缓冲液，采用梯度洗脱。黄连素采用电喷雾电离-质谱（ESI-MS）测定。LC-ESI-MS在选择离子监测（SIM）模式下进行，黄连素的目标离子为m/z 336.1的M(+)，内标的目标离子为m/z 464.1的M(+)。校准曲线在0.020 - 3.0 ng/ml范围内呈线性。定量下限（LLOQ）为0.020 ng/ml。批内和批间变异值分别小于6.7%和7.7%。该方法已成功应用于测定健康中国志愿者血浆中黄连素的浓度。
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