Department of Pharmaceutical Analysis and Metabolomics, Jiangsu Province Academy of Traditional Chinese Medicine, Nanjing 210028, PR China; Department of Chinese Medicines Analysis, China Pharmaceutical University, Nanjing 210009, PR China.
J Pharm Biomed Anal. 2014 Jan;88:391-400. doi: 10.1016/j.jpba.2013.09.023. Epub 2013 Oct 6.
A high performance liquid chromatography-photodiode array detector (HPLC-PDA) fingerprinting and ultra high performance liquid chromatography-photodiode array detector coupled with quadrupole time-of-flight mass spectrometry (UHPLC-PDA-QTOF-MS/MS) based chemical profiling approach was developed to rapidly find characteristic chemical markers for quality control of dispensing granules, taking Chuanxiong Rhizoma (CR) as a model herb. Firstly, CR crude drugs, their traditional decoctions and CR dispensing granules were analyzed by HPLC-PDA to rapidly establish the fingerprints and thereby generate the simulative median chromatograms of CR crude drugs, decoctions and dispensing granules, and by comparing the simulative median chromatograms, major characteristic peaks of CR decoctions and dispensing granules could be determined. Secondary, UHPLC-PDA-QTOF-MS/MS was used to identify the major characteristic peaks of CR decoctions and dispensing granules. The identities of three major peaks were elucidated and confirmed to be ferulic acid (1), senkyunolide I (2) and senkyunolide H (3) by comparing the mass/UV spectra and retention times with that of the reference compounds. Thirdly, an HPLC-PDA method was validated to quantify the three characteristic components in commercial CR dispensing granules. The average contents of ferulic acid and senkyunolide H were found to be less than 1.0mg/g, whereas that of senkyunolide I was 4.40mg/g in CR dispensing granules, which indicated that senkyunolide I might be chosen as a suitable quantitative marker, while ferulic acid and senkyunolide H as qualitative markers for the quality evaluation of CR dispensing granules. It is suggested that this newly established approach could be used to practically and rapidly find suitable marker compounds for quality control of dispensing granules derived from other medicinal herbs.
建立了高效液相色谱-光电二极管阵列检测（HPLC-PDA）指纹图谱和超高效液相色谱-光电二极管阵列检测与四级杆飞行时间质谱联用（UHPLC-PDA-QTOF-MS/MS）的化学分析方法，以川芎（CR）为模型草药，快速寻找特征性化学标志物，用于调配颗粒的质量控制。首先，采用 HPLC-PDA 对 CR 生药、传统汤剂和 CR 调配颗粒进行分析，快速建立指纹图谱，并生成 CR 生药、汤剂和调配颗粒的模拟中值色谱图，通过比较模拟中值色谱图，确定 CR 汤剂和调配颗粒的主要特征峰。其次，采用 UHPLC-PDA-QTOF-MS/MS 鉴定 CR 汤剂和调配颗粒的主要特征峰。通过比较质量/紫外光谱和保留时间，确定了三个主要峰的结构，并确认为阿魏酸（1）、川芎嗪 I（2）和川芎嗪 H（3）。第三，建立了 HPLC-PDA 方法对商业 CR 调配颗粒中的三种特征成分进行定量分析。结果发现，阿魏酸和川芎嗪 H 的平均含量均低于 1.0mg/g，而川芎嗪 I 的含量为 4.40mg/g，表明川芎嗪 I 可能被选为合适的定量标志物，而阿魏酸和川芎嗪 H 则作为 CR 调配颗粒质量评价的定性标志物。建议将该新建立的方法应用于从其他草药中实际快速寻找合适的标记化合物，以控制调配颗粒的质量。
