Su Meng-xiang, Zhou Wen-di, Lan Juan, Di Bin, Hang Tai-jun
Department of Pharmaceutical Analysis, China Pharmaceutical University, Nanjing, P. R. China; Key Laboratory of Drug Quality Control and Pharmacovigilance (China Pharmaceutical University), Ministry of Education, Nanjing, P. R. China.
J Sep Sci. 2015 Mar;38(5):804-12. doi: 10.1002/jssc.201400946. Epub 2015 Jan 27.
A simultaneous determination method based on liquid chromatography coupled with time-of-flight mass spectrometry was developed for the analysis of 11 bioactive constituents in tripterygium glycosides tablets, an immune and inflammatory prescription used in China. The analysis was fully optimized on a 1.8 μm particle size C18 column with linear gradient elution, permitting good separation of the 11 analytes and two internal standards in 21 min. The quantitation of each target constituent was carried out using the narrow window extracted ion chromatograms with a ±l0 ppm extraction window, yielding good linearity (r(2) > 0.996) with a linear range of 10-1000 ng/mL. The limits of quantitation were low ranging from 0.25 to 5.02 ng/mL for the 11 analytes, and the precisions and repeatability were better than 1.6 and 5.3%, respectively. The acceptable recoveries obtained were in the range of 93.4-107.4%. This proposed method was successfully applied to quantify the 11 bioactive constituents in commercial samples produced by nine pharmaceutical manufacturers to profile the quality of these preparations. The overall results demonstrate that the contents of the 11 bioactive constituents in different samples were in great diversity, therefore, the quality, clinical safety, and efficacy of this drug needs further research and evaluation.
建立了一种基于液相色谱-飞行时间质谱联用的同时测定方法，用于分析中国一种免疫和炎症处方雷公藤多苷片中的11种生物活性成分。在1.8μm粒径的C18柱上采用线性梯度洗脱对分析进行了全面优化，可在21分钟内实现11种分析物和两种内标的良好分离。使用±10 ppm提取窗口的窄窗口提取离子色谱图对每种目标成分进行定量，线性良好（r(2)>0.996），线性范围为10 - 1000 ng/mL。11种分析物的定量限较低，范围为0.25至5.02 ng/mL，精密度和重复性分别优于1.6%和5.3%。获得的可接受回收率在93.4%至107.4%范围内。该方法成功应用于九家制药企业生产的市售样品中11种生物活性成分的定量分析，以表征这些制剂的质量。总体结果表明，不同样品中11种生物活性成分的含量差异很大，因此，该药物的质量、临床安全性和疗效需要进一步研究和评估。
