State Key Laboratory of Natural Medicines (China Pharmaceutical University), No. 24 Tongjia Lane, Nanjing 210009, China.
Analyst. 2013 Apr 21;138(8):2279-88. doi: 10.1039/c3an36732k.
In this work, a rapid and simple method based on matrix solid-phase dispersion (MSPD) and ultra performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS) was developed. Guge Fengtong preparation (GGFT), a traditional Chinese herbal medicine, was investigated for validation, and eight major constituents were determined including four saponins (protodioscin, protogracillin, pseudoprotodioscin and dioscin) and four gingerols (6-gingerol, 8-gingerol, 10-gingerol and 6-shogaol). Response surface methodology and desirability function were employed to optimize the extraction conditions, such as dispersant, dispersant/sample ratio, solvent concentration, and elution volume, of MSPD. Results showed that MSPD using C18 (1.75 g) as the dispersant material and methanol (89%, v/v) as the eluting solvent (12.00 mL) resulted in a high extraction efficiency. MSPD extraction had the advantages of combining extraction and clean-up in a single step, was less time consuming and required lower solvent volumes compared with conventional methods. Quantification of chemical compounds from GGFT preparations were performed using UPLC-MS/MS in multiple-reaction monitoring mode. The proposed method afforded a low limit of detection ranging from 0.02 to 0.40 ng for saponins and gingerols. For all the analytes, recoveries ranged from 80.9% to 103% and repeatabilities were acceptable with relative standard deviations of less than 6.81%. The proposed MSPD-UPLC-MS/MS method was successfully utilized to analyze five batches of GGFTs, and the results demonstrated that this method is simple, efficient and has potential to be applied for the quality control of herbal preparations.
在这项工作中,建立了一种基于基质固相分散(MSPD)和超高效液相色谱-串联质谱(UPLC-MS/MS)的快速简单方法。古格丰通制剂(GGFT)是一种中药,对其进行了验证,测定了包括四种皂甙(原薯蓣皂甙、原薯蓣皂甙、伪原薯蓣皂甙和薯蓣皂甙)和四种姜酚(6-姜酚、8-姜酚、10-姜酚和 6-姜辣素)在内的八种主要成分。采用响应面法和适宜性函数优化 MSPD 的提取条件,如分散剂、分散剂/样品比、溶剂浓度和洗脱体积。结果表明,MSPD 采用 C18(1.75 g)作为分散剂材料,甲醇(89%,v/v)作为洗脱溶剂(12.00 mL),提取效率较高。MSPD 提取具有在单个步骤中结合提取和净化的优点,与常规方法相比,耗时更少,所需溶剂体积更小。采用 UPLC-MS/MS 多反应监测模式对 GGFT 制剂中的化合物进行定量分析。所提出的方法对皂甙和姜酚的检测限低至 0.02-0.40 ng。对于所有分析物,回收率在 80.9%-103%之间,重复性好,相对标准偏差小于 6.81%。所提出的 MSPD-UPLC-MS/MS 方法成功地用于分析五批 GGFT,结果表明该方法简单、高效,具有应用于草药制剂质量控制的潜力。