Analysis of Specific Chromatogram of Wenjingtang Reference Sample / 中国实验方剂学杂志

Objective:To control the quality of the reference sample of Wenjingtang by establishing the specific chromatograms. Method:On the basis of analyzing 15 batches of Wenjingtang freeze-dried powder samples， a high performance liquid chromatography （HPLC） specific chromatogram analysis method of Wenjingtang was established. The system adaptability was investigated and the retention time， relative retention value and deviation caused by different chromatographic columns and instruments were calculated by using the same brand of chromatographic columns， four different brands of chromatographic columns and instruments from three different manufacturers. The precision， repeatability and stability of this method was further completed. The possible chemical components of the freeze-dried powders were speculated and identified by ultra-performance liquid chromatography-quadrupole-time-of-flight mass spectrometry （UPLC-Q-TOF-MS<italic>ⁿ</italic>）. Chromatographic separation was performed on ACQUITY UPLC BEH C₁₈ column （2.1 mm×100 mm， 1.7 μm） with acetonitrile （A）-0.1% formic acid aqueous solution （B） as mobile phase for gradient elution （0-2.8 min， 10%A； 2.8-8.0 min， 10%-18%A； 8.0-12.2 min， 18%-25%A； 12.2-15.3 min， 25%-40%A； 15.3-17.4 min， 40%A； 17.4-20.5 min， 40%-90%A）， and column temperature was set at 30 ℃ with flow rate of 0.4 mL·min^-1. Mass spectrometry was performed on electrospray ionization， data were collected under positive and negative ion modes， and the detection range was <italic>m</italic>/<italic>z</italic> 50-1 600. Result:Ten characteristic peaks were selected as the distinguishing features in this specific chromatograms， and eight of them were identified by comparing with the reference standards， including paeoniflorin （peak 1）， liquiritin apioside （peak 2）， liquiritin （peak 3）， ferulic acid （peak 4）， iquiritigenin （peak 6）， cinnamaldehyde （peak 8）， paeonol （peak 9）and glycyrrhizic acid （peak 10）. By mass spectrometry analysis， 30 compounds were identified， and the source of medicinal materials were assigned. It mainly contained triterpenoid saponins and flavonoids from Glycyrrhizae Radix et Rhizoma， ginsenosides from Ginseng Radix et Rhizoma， monoterpenoid glycosides and tannins from Paeoniae Radix Alba， steroids in Achyranthis Bidentatae Radix， phenolic acids in Angelicae Sinensis Radix. Conclusion:The established characteristic chromatographic analysis method of Wenjingtang is simple， stable and repeatable. The chemical composition of the freeze-dried powder of Wenjingtang is basically defined by mass spectrometry identification and source attribution， which can provide reference for the development and quality control of Wenjingtang in the future.

Identification of Gastrodiae Rhizoma chromatographic peaks identification by liner calibration with two reference substances assisted / 药学学报

This study aimed to establish a method for positioning six chromatographic peaks occurred in HPLC profile of Gastrodiae Rhizoma. The "liner calibration with two reference substances" (LCTRS) method was used to calculate the retention time so as to assist in positioning of chromatographic peaks in terms of the prediction accuracy of retention time and the coincidence rate of chromatographic column. A total of 24 C18 chromatographic columns from different brands and types available were used to determine the retention times of six components in Gastrodiae Rhizoma, then the average retention time of each component was obtained as standard retention time (SRT). Parishin E (peak 3) and Parishin A (peak 6) were simultaneously taken as reference substance to forecast the retention time of the other four components by using the LCTRS method. Four different C18 columns were employed to verify the method. Meanwhile, for the purpose of comparison, the relative retention time (RRT) method was applied to forecast the retention time, by using Parishin E as the single reference substance. The comparison between LCTRS and RRT methods indicated that the former was more accurate in predicting the retention time and more applicable in utilization of chromatographic columns. This study demonstrated that the LCTRS method shows the superior performance in positioning of chromatographic peak, and therefore has a good prospect of application.

Study on UHPLC Fingerprints of Psoralea corylifolia L / 世界科学技术-中医药现代化

This study was aimed to establish the ultra high performance liquid chromatography (UHPLC) fingerprints of Psoralea corylifolia L. The separation was achieved on a Shim-pack XR-ODS Ⅲ column (50 mm í 2.0 mm, 1.6μm) by gradient elution with acetonitrile-0.2% glacial acetic acid solution as the mobile phase. The flow rate was 0.1 mL·min-1 and the measurement wavelength was 246 nm. The temperature of the column was 45oC. The results showed that the UHPLC fingerprint of P. corylifolia L. was established and 10 characteristic common peaks were found, among which 6 peaks were recognized by comparing with reference substances. It was concluded that the method was rapid, reliable and reproducible. The established fingerprint can provide references for the study of sub-stance basis and quality control of P. c orylifolia L.