Using the HPLC/DAD/ESI/MS method, the qualitative and quantitative analysis of senkyunolide A (SA) in the rhizomes of Ligusticum chuanxiong (Rhizoma chuanxiong; CX) and roots of Angelica sinensis (DG) was established. As a result, it was found that SA is a characteristic standard compound for the quality evaluation and chemical differentiation between CX and DG. Methanol was chosen in the preparation of standard solutions and extraction of samples based on the stability data. The identity of SA in CX and DG was unambiguously determined based on the quasimolecular ions in ESI-MS. A comprehensive validation of the method, including sensitivity, linearity, reproducibility and recovery, was conducted using the optimized chromatographic conditions. The linear calibration curve was acquired with R2>0.999 and limit of detection (S/N=3) was estimated to be 12.5 mug/g. The reproducibility was evaluated by repeated sample injection and replicated analysis of samples with the relative standard deviation (RSD) value found within 0.68%. The recovery rates of SA varied within the range of 96.91-101.50% with RSD less than 2.38%. In the present work, the contents of SA were quantified within 3.94-9.14 mg/g and 0.108-0.588 mg/g for 12 batches each of CX and DG. The results demonstrated that SA is a useful standard compound for the quality evaluation and chemical differentiation between CX and DG. The analytical procedure is precise and reproducible and thus suitable for the analysis of a large number of samples.
"ASR and CR both belong to the Apiaceae family, and are quite similar in their chemical constituents, including phthalides (e.g., Z-ligustilide, senkyunolide A, butylphthalide and Z-butylidenephthalide) and phenolic compounds (e.g., ferulic acid and coniferyl ferulate) . Wine treatment of ASR and CR is a commonly adopted procedure. "
[Show abstract][Hide abstract] ABSTRACT: Background
Angelicae Sinensis Radix (ASR) and Chuanxiong Rhizoma (CR) can be treated with wine to promote their biological functions in Chinese medicine. Both ASR and CR contain similar volatile chemicals that could be altered after wine treatment. This study aims to identify the differential chemical profiles and to select marker chemicals of ASR and CR before and after wine treatment.
Chemical analyses were carried out by gas chromatography-triple quadrupole mass spectrometry (GC-QQQ-MS/MS) coupled with multivariate statistical analysis. Characterization of the compositions of essential oils was performed by automated matching to the MS library and comparisons of their mass spectra (NIST08 database). For ferulic acid, butylphthalide, Z-butylidenephthalide, senkyunolide A and Z-ligustilide, the mass spectrometer was operated in electron ionization mode, the selection reaction monitoring mode was used and an evaluation of the stability and sensitivity of the chromatographic system was performed for the tested extraction.
Principal component analysis (PCA) simultaneously distinguished ASR and CR from different forms. Ferulic acid, Z-butylidenephthalide, Z-ligustilide, butylphthalide and senkyunolide A were screened by PCA loading plots and can be used as chemical markers for discrimination among different groups of samples.
Different chemical profiles of ASR and CR after wine treatment could be identified by GC-QQQ-MS/MS. The five marker chemicals selected by PCA, namely ferulic acid, butylphthalide, Z-butylidenephthalide, senkyunolide A and Z-ligustilide, were sufficient to distinguish between the crude and corresponding wine-treated forms of ASR and CR.
Chinese Medicine 06/2013; 8(1):12. DOI:10.1186/1749-8546-8-12 · 1.49 Impact Factor
[Show abstract][Hide abstract] ABSTRACT: An HPLC-DAD-MS method was developed for the qualitative and quantitative analysis of the major constituents in Chuanxiong (the dried rhizome of Ligusticum chuanxiong Hort). Twenty compounds including phenolic constituents, alkylphthalides and phthalide dimers were identified using online ESI-MS and comparisons with literature data and standard compounds, and six of them were quantified by HPLC-DAD simultaneously. A comprehensive validation of the method including sensitivity, linearity, repeatability and recovery was conducted. The linear regressions were acquired with R(2) > 0.99 and limit of detection (LOD, S/N = 3) values were between 1.5 and 2.5 ng. The repeatability was evaluated by intra- and inter-day assays, and relative standard deviation (RSD) values were reported within 1.87%. The recovery studies for the quantified compounds were observed in the range of 96.36-102.37% with RSD values less than 2.63%. These phenolic constituents and alkylphthalides, the major constituents in Chuanxiong, are generally regarded as the index for the quality assessment of this herb. The overall procedure is accurate and reproducible, which is considered suitable for the qualitative and quantitative analyses of a large number of Chuanxiong samples.
[Show abstract][Hide abstract] ABSTRACT: An high performance liquid chromatography (HPLC) coupled with diode array detector (DAD) and electrospray ionization tandem mass spectrometry (ESI/MS(n)) method was developed for quality evaluation of Cortex Moutan through identification of common constituents based on chromatographic fingerprints and determination of key pharmacological compounds. The representative chromatographic fingerprints of Cortex Moutan were obtained by analyzing 10 batches of samples under the optimized HPLC conditions and the results showed that the chromatographic profiles of the analyzed samples were very similar. Total of nineteen common peaks were detected and seventeen of them were identified rapidly by their characteristic UV profile and the information of molecular structure provided by ESI/MS(n) experiments. Simultaneously, five key pharmacological compounds, namely gallic acid, oxypaeoniflorin, paeoniflorin, benzoylpaeoniflorin and paeonol, were determined by the validated HPLC-DAD method. The linear calibration curves were acquired with correlation coefficients higher than 0.999. The precisions of intra-day and inter-day were not exceeding 3.1%, and the recoveries of five analytes were from 92.86 to 99.35%. This developed method that combined the chromatographic fingerprints and quantification assay ensured the phytoequivalence and pharmacological effects of Cortex Moutan and was successfully applied to the quality control of Cortex Moutan.
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