Xu Beilei, Li Pengyue, Zhang Guijun
Research Center on Life Sciences and Environmental Sciences, Harbin University of Commerce, Harbin 150076, Heilongjiang, China; School of Pharmacy, Harbin University of Commerce, Harbin 150076, Heilongjiang, China.
Institute of Chinese Materia Medica, China Academy of Chinese Medical Sciences, Beijing 100700, Beijing, China.
J Chromatogr B Analyt Technol Biomed Life Sci. 2015 Apr 15;988:33-44. doi: 10.1016/j.jchromb.2015.01.039. Epub 2015 Feb 17.
An LC-MS/MS method was developed for simultaneous analysis of puerarin, daidzin, baicalin, glycyrrhizic acid, liquiritin, berberine, palmatine and jateorhizine of Gegenqinlian Decoction (GQD) and active components alignment (ACA) in rat plasma using hesperidin as the internal standard (I.S.). Chromatography was performed using a C18 column, with gradient elution with 1% acetic acid-0.001 mol/L ammonium acetate and acetonitrile at 0.2 ml/min. All analytes including I.S. were monitored under positive ionization conditions by selected reaction monitoring with an electrospray ionization source. The optimized mass transition ion-pairs (m/z) for quantitation were 471/297 for puerarin, 471/255 for daidzin, 447/271 for baicalin, 823/453 for glycyrrhizic acid, 419/257 for liquiritin, 336/320 for berberine, 352/336 for palmatine, 338/322 for jateorhizine and 611/303 for hesperidin. The calibration curves were linear over the concentration ranges from 0.15-63.0 to 6.3-6340.0 ng/mL. Intra-day and inter-day precisions (RSD%) were within 15.0%, and accuracy (RE%) ranged from -7.4 to 13.2%. The extraction recoveries were ranged from 60.4 to 93.3%. The proposed method was further applied to compare the pharmacokinetics of all analytes following a single oral administration of GQD and ACA. In conclusion, the eight analytes of GQD and ACA had partly similar pharmacokinetics, which were different from single composition (such as puerarin).
建立了一种液相色谱-串联质谱(LC-MS/MS)方法,以橙皮苷为内标,同时分析葛根芩连汤(GQD)中的葛根素、大豆苷、黄芩苷、甘草酸、甘草苷、小檗碱、巴马汀和jatrorhizine以及大鼠血浆中的活性成分比对(ACA)。采用C18柱进行色谱分析,以1%乙酸-0.001 mol/L乙酸铵和乙腈进行梯度洗脱,流速为0.2 ml/min。所有分析物(包括内标)在正离子化条件下通过电喷雾电离源的选择反应监测进行监测。用于定量的优化质量转移离子对(m/z)分别为:葛根素471/297、大豆苷471/255、黄芩苷447/271、甘草酸823/453、甘草苷419/257、小檗碱336/320、巴马汀352/336、jatrorhizine 338/322、橙皮苷611/303。校准曲线在0.15 - 63.0至6.3 - 6340.0 ng/mL的浓度范围内呈线性。日内和日间精密度(RSD%)在15.0%以内,准确度(RE%)在-7.4至13.2%之间。提取回收率在60.4%至93.3%之间。所提出的方法进一步应用于比较单次口服GQD和ACA后所有分析物的药代动力学。总之,GQD和ACA的八种分析物具有部分相似的药代动力学,这与单一成分(如葛根素)不同。