ABSTRACT
OBJECTIVE To establi sh the fingerprint of Cnidium monnieri and a method for the content determination of 4 kinds of coumarins. METHODS Ultra-high performance liquid chromatography （UPLC） method was adopted to establish the fingerprints of 21 batches of C. monnieri ； their similarities were evaluated with Similarity Evaluation System of TCM Chromatographic Fingerprint （2012 edition）；common peaks were identification by comparison with reference substance. Using 10 common peak areas as variables ，cluster analysis was performed for 21 batches of C. monnieri by the method of between groups. The relative correction factors of xanthotoxin ，bergapten and imperatorin were calculated by the same UPLC method with osthole as the internal reference. The contents of them were calculated by quantitative analysis of multi-components by single marker （QAMS），and compared with the results of external standard method. RESULTS Totally 10 common peaks were identified in the fingerprints of 21 batches of C. monnieri ；the similarities ranged from 0.997 to 1.000. Peak 4 was identified as xanthotoxin ，peak 8 as bergapten ，peak 9 as imperatorin and peak 10 as osthole. A total of 21 batches of samples were divided into 3 categories，of which S 7 was clustered into one category ，S14 was clustered into one category ，and the other 19 batches were clustered into one category. The relative deviations of the contents of xanthotoxin ，bergapten and imperatorin determined by QAMS and external standard method were in the range of 0.88％ -1.07％ ，2.22％ -2.29％ ，0.67％ -2.93％ ，respectively. CONCLUSIONS UPLC fingerprint of C. monnieri is successfully established ，and QAMS method for content determination of 4 coumarins is also established.
ABSTRACT
Objective:To establish the quality evaluation method of Prunellae spica dispensing granules based on three quality indexes of standard decoction. Methods:Fourteen batches of Prunellae spica were collected from different habitats. According to technical requirements, fourteen batches of Prunellae spica standard decoction and three batches of formula granules were prepared and the paste-forming rates were calculated. The fingerprints of Prunellae spica standard decoction and formula granules were established by Ultra High Performance Liquid Chromatography (UPLC). The similarity values of fingerprints between dispensing granules and standard decoction were calculated. The content and transferring rate of Rosmarinic acid were determined and calculated. Results:The average paste-forming rate of Prunellae spica was (12.59±2.32)%. The paste-forming rates of the three batches were 11.14%, 10.78% and 10.39% respectively. The average content of Rosmarinic acid in standard decoction was (18.99±9.74)mg/g. The average transferring rate was (60.58±7.87)%. The contents of three batches were 7.40 mg/g, 7.49 mg/g and 7.09 mg/g. The transferring rates were 52.06%, 50.10% and 50.40% respectively. Nine common fingerprint peaks were identified in the fingerprints of standard decoction and formula granules, two of which were identified as Rosmarinic acid and Caffeic acid by comparison of reference substance. The fingerprints similarity of Prunellae spica dispensing granules and standard decoction were 0.954, 0.973 and 0.952, respectively. Conclusions:The quality indexes of three batches of formulation granules are consistent with standard decoction. This method could provide reference for the establishment of quality standard of Prunellae spica dispensing granules.
ABSTRACT
OBJECTIVE：To compare the chemical components in Sinapis alba before and after stir-frying. METHODS ： UPLC-Q-Exactive Obitrap MS was adopted to analyze chemical constituents of S. alba before and after stir-frying. The determination was performed on Waters CORTECS T 3 column with mobile phase consisted of methanol- 0.1％ formic acid solution （gradient elution ）at the flow rate of 0.25 mL/min. The column temperature was 30 ℃ and the sample size was 2 μL. High resolution MS adopted heating electrospray electron source ，positive ion scanning mode ，scanning range m/z 120-1 000. The chemical constituents of S. alba before and after stir-frying were identified by Compound Discover 3.2 software combined with relevant database ，and the content changes of chemical constituents were analyzed by using peak area. Chemometrics analysis was performed for the content changes of chemical constituents using peak area as variable. RESULTS ：A total of 54 chemical components were identified in S. alba ，mainly fatty acids （represented by erucic acid ），alkaloids（represented by sinapine ）， flavonoids. After stir-frying ，the contents of 19 chemical components changed significantly ，of which the contents of 10 components decreased significantly and those of 9 components increased significantly （P＜0.05）. Principal component analysis and orthogonal partial least squares discriminant analysis could clearly distinguish S. alba from stir-fried S. alba . CONCLUSIONS ：The contents of some chemical components of S. alba change significantly after stir-frying ，which may be one of the important reasons for the change of efficacy after stir-frying.