Wang Jin, Zhang Hai-Hong, Tian Jia-Ming, Liu Feng-Xi, Zhang Yu-Ping, Zhao Yong-Ming
Department of Pharmacy, Hebei North University, Zhangjiakou, P.R. China.
Hebei Key Laboratory of Neuropharmacology, Zhangjiakou, China.
Biomed Chromatogr. 2019 Dec;33(12):e4677. doi: 10.1002/bmc.4677. Epub 2019 Sep 2.
An efficient ultra-performance liquid chromatography with diode-array detector method was established for simultaneous determination of six active components in Roukou Wuwei pills, namely gallic acid, piperine, costundide, dehydrocostus lactone, isoalantolactone and alantolactone. Chromatographic separation of six components was successfully achieved on an Waters BEH C column (50 × 2.1 mm, 1.7 μm) with a mobile phase composed of acetonitrile and water using a gradient elution. Gallic acid and piperine were detected at 270 nm and 343 nm, respectively; while costundide, dehydrocostus lactone, isoalantolactone and alantolactone were simultaneously measured at 225 nm. All six calibration curves showed good linearity (R ≥ 0.9994) between the peak area of each component and corresponding concentration. Relative standard deviations for inter- and intra-day precisions were <0.45 and 0.77%, respectively. The mean recovery rates ranged from 96.72 to 102.2% with relative standard deviations <2.07%. The developed method was validated in terms of linearity, precision and accuracy and then successfully applied for the quality control of commercial Roukou Wuwei samples.
建立了一种高效液相色谱-二极管阵列检测法，用于同时测定肉蔻五味丸中的六种活性成分，即没食子酸、胡椒碱、木香烃内酯、去氢木香内酯、异土木香内酯和土木香内酯。六种成分在Waters BEH C18柱（50×2.1 mm，1.7μm）上成功实现色谱分离，流动相由乙腈和水组成，采用梯度洗脱。没食子酸和胡椒碱分别在270 nm和343 nm波长处检测；而木香烃内酯、去氢木香内酯、异土木香内酯和土木香内酯在225 nm波长处同时测定。所有六种校准曲线在各成分峰面积与相应浓度之间均显示出良好的线性关系（R≥0.9994）。日内和日间精密度的相对标准偏差分别<0.45%和0.77%。平均回收率在96.72%至102.2%之间，相对标准偏差<2.07%。所建立的方法在线性、精密度和准确度方面得到验证，然后成功应用于市售肉蔻五味丸样品的质量控制。
