Zhao Minmin, Ding Weijing, Wang Shuang, Gao Meng, Fu Shan, Zhang Juan, Li Tao, Wu Yin, Wang Qiao
Department of Pharmaceutical Analysis, School of Pharmacy, Hebei Medical University, 361 East Zhongshan Road, Shijiazhuang 050017, P.R. China.
Department of Pharmaceutical Analysis, School of Pharmacy, Hebei Medical University, 361 East Zhongshan Road, Shijiazhuang 050017, P.R. China
J Chromatogr Sci. 2015 Feb;53(2):274-9. doi: 10.1093/chromsci/bmu052. Epub 2014 Jun 11.
A rapid high-performance liquid chromatography coupled with tandem mass spectrometry method was developed for the simultaneous determination of five constituents in Qinpijiegu capsule (QJC), a classical Tibetan prescription. The separation of five compounds such as aesculin, aesculetin, fraxin, peimine and peiminine was performed on a Purospher STAR LP RP-C18 (250 × 4.6 mm, 5 μm) column with linear gradient elution of acetonitrile-0.3‰ formic acid water in 13 min. Detection was carried out by multiple reaction monitoring mode using electrospray ionization in the positive and negative ion switching mode. The sample was prepared with ultrasound extraction with methanol, which could obtain higher extraction efficiency and shorter extraction time comparing to reflux extraction with alkalized chloroform-methanol. The proposed method was applied to analyze three batches of samples with acceptable linearity (r(2) > 0.9977), precision [relative standard deviation (RSD) < 7.40%], repeatability (RSD < 2.49%), stability [relative error (RE) < 9.15%] and recovery (RSD < 10.76%). This is the first development of a multicomponent quantitation method for the quality control of QJC. Furthermore, the new established method was proven to be highly sensitive and effective in evaluating the quality of QJC.
建立了一种快速高效液相色谱-串联质谱法,用于同时测定经典藏药方剂秦皮接骨胶囊(QJC)中的五种成分。采用Purospher STAR LP RP-C18(250×4.6 mm,5μm)色谱柱,以乙腈-0.3‰甲酸水进行线性梯度洗脱,在13分钟内分离七叶苷、七叶内酯、秦皮素、贝母碱和去氢贝母碱等五种化合物。采用电喷雾电离,在正、负离子切换模式下通过多反应监测模式进行检测。样品采用甲醇超声提取制备,与碱化氯仿-甲醇回流提取相比,提取效率更高,提取时间更短。该方法应用于三批样品的分析,线性关系良好(r(2)>0.9977),精密度[相对标准偏差(RSD)<7.40%],重复性(RSD<2.49%),稳定性[相对误差(RE)<9.15%]和回收率(RSD<10.76%)。这是首次开发用于QJC质量控制的多组分定量方法。此外,新建立的方法在评估QJC质量方面被证明具有高灵敏度和有效性。