建立了超高效液相色谱串联质谱法测定大鼠灌胃给予参松养心胶囊后胆汁中的芍药苷、斯皮诺素和五味子甲素。采用Waters UPLC C18 色谱柱,乙腈-0.1%甲酸为流动相,梯度洗脱,正离子多反应监测(MRM)。芍药苷、斯皮诺素和五味子甲素分别在24.6 ~ 1 720、28.6 ~ 1 430 和2.8 ~ 700 ng/ml 范围内线性关系良好,提取回收率为88.7%~100.9%,基质效应为91.28%~ 102.70%,日内和日间RSD 均小于6.22%,相对误差为-6.58 ~ 7.51%。
Abstract
An UPLC-MS/MS method was established for the determination of paeoniflorin, spinosin and deoxyschizandrin in rat bile after intragastric administration of Shensong Yangxin capsules. A Waters UPLC C18 column was used with the mobile phase of acetonitrile-0.1% formic acid by gradient elution. Electrospray ionization (ESI) source was employed and the three analytes were detected by multiple reaction monitoring (MRM) scanning under the positive ionization mode. The calibration curves for paeoniflorin, spinosin and deoxyschizandrin were linear in the concentration ranges of 24.6 - 1 720, 28.6 - 1 430 and 2.8 - 700 ng/ml, respectively. Their extraction recoveries were 88.7% - 100.9% and the matrix effects were 91.28% - 102.70% in rat bile. The intra- and inter-day RSDs were less than 6.22% with the relative errors (RE) within -6.58% to 7.51%.
关键词
参松养心胶囊 /
芍药苷 /
斯皮诺素 /
五味子甲素 /
胆汁 /
超高效液相色谱串联质谱 /
测定
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Key words
Shensong Yangxin capsules /
paeoniflorin /
spinosin /
deoxyschizandrin /
bile /
UPLC-MS/MS /
determination
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参考文献
[1] 陈汉想, 郭秋慧, 刘 立, 等. 参松养心胶囊预防垂体后叶素致实验性大鼠急性心肌缺血的研究[ J] . 中国医院药学杂志, 2007, 27(11): 1520-1522.
[2] 任景怡, 李丽君, 汪若婕, 等. 参松养心胶囊对大鼠心肌缺血/ 再灌注后室性心律失常的影响[ J] . 中华医学杂志, 2008, 88(48): 3440-3443.
[3] 李 宁, 吴相锋, 马克娟, 等. 参松养心胶囊对心室肌细胞钾通道的影响[J]. 疑难病杂志, 2007, 6(3): 133-137.
[4] 石 亮, 杨新春, 刘秀兰, 等. 参松养心胶囊干粉提取液对兔肺静脉肌袖心肌细胞动作电位和部分离子通道的影响[J]. 中华医学杂志, 2009, 89(30): 2142-2146.
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脚注
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基金
国家科技重大专项课题(2011ZX09201-201-28)、国家重点基础研究发展计划(973计划)项目(2012CB518606)
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