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Objective:To comprehensively evaluated the quality of Sargentodoxae Caulis from different habitats with a combination of indexes and characteristic chromatogram method from Chinese Pharmcopoeia (Edition 2020). Methods:The contents of water content, total ash, ethanolic extract, sulfur dioxide residue, heavy metals and harmful elements, total phenols, chlorogenic acid, salidroside and characteristic chromatogram of 17 batches of Sargentodoxae Caulis were determined. The quality of Sargentodoxae Caulis was comprehensively evaluated by combining chemical pattern recognition method. Results:The water content, total ash content, extracts, and content determination of 17 batches of Sargentodoxae Caulis from different habitats complyed with the provisions of the Chinese Pharmcopoeia (Edition 2020). There were differences in the contents of extracts, chlorogenic acid, and salidroside, among which the content of Anhui origin was higher. A total of 8 common peaks were identified from the 17 batches samples. Conclusion:Comprehensive evaluation of multiple indicators can demonstrate the quality of Sargentodoxae Caulis more correctly, and shows that the quality of Sargentodoxae Caulis from different habitats is different. The quality of Sargentodoxae Caulis from Anhui is better than that from other habitats.
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Objective:To establish the quality evaluation method of Perillae caulis formula granules based on the three kind of quality indexes of standard decoction. Methods:Eighteen batches of Perillae caulis were collected from different habitats according to different technical requirements, eighteen batches of standard decoction and three batches of formula granules were prepared and the paste-forming rates were calculated. The content of Caffeic acid and Rosmarinic acid were determined and calculated by Ultra High Performance Liquid Chromatography (UPLC). Then the fingerprints of standard decoction of and formula granules of Perillae caulis were established by UPLC . The similarity values of fingerprints between formula granules and standard decoction were calculated. Results:The average paste-forming rate of standard decoction was (7.16±1.97)%. The paste-forming rates of three batches of formula granules were 5.52%, 5.25% and 5.34%, respectively. The average content of Caffeic acid and Rosmarinic acid in standard decoction was (12.06±3.37)mg/g. The contents of three batches of formula granules were 5.52, 5.82, 5.77 mg/g, respectively. Seven common fingerprint peaks were identified in the fingerprints of standard decoction and formula granules, three of which were identified as Caffeic acid, N-Feruloyl Octopus amine and Rosmarinic acid by comparison of reference substance. The fingerprints similarity of Perillae caulis dispensing granules and standard decoction were 1.000, 0.995 and 0.997, respectively. Conclusions:The quality indexes of three batches of formulation granules are consistent with standard decoction. This method can provide basis for the establishment of quality standard of Perillae caulis dispensing granules.
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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.
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OBJECTIVE:To establish the UPLC fingerprint of Polygonum cuspidatum ,and to determine the contents of four active ingredients and to provide reference for the quality evaluation of P. cuspidatum . METHODS :The determination was performed on Waters BEH C 18 column(100 mm×2.1 mm,1.7 μm)with mobile phase consisted of acetonitrile- 0.2% formic acid (gradient elution )at flow rate of 0.4 mL/min. The column temperature was 40 ℃,and detection wavelength was 290 nm. The sample size was 1 μL. The fingerprints were evaluated by similarity calculation,cluster analysis and orthogonal partial least square discriminant analysis (OPLS-DA). Using polydatin as internal standard ,relative calibration factors of resveratrol ,emodin-8-O- β-D-glucoside and emodin were determined to develop a method of QAMS. The contents of 4 above components in 15 batches of P. cuspidatum were calculated by relative calibration factors. The results of QAMS were compared with those of external standard. RESULTS:UPLC fingerprints of 15 batches of P. cuspidatum were established ,and 12 common peaks were confirmed. Five components were identified ,i.e. polydatin ,resveratrol,emodin-8-O-β-D-glucoside,emodin,emodin methyl ether. The fingerprint similarity of 15 batches of P. cuspidatum was in the range of 0.865-0.976. According to cluster analysis ,15 batches of P. cuspidatum were classified into 4 categories,showing certain regularity of origin. Seven markers were identified by OPLS-DA method. The order of difference significance was peak 7>emodin-8-O-β-D-glucoside>resveratrol>peak 8>polydatin>peak 1> peak 10. The relative deviation among the contents of resveratrol ,emodin-8-O-β-D-glucoside and emodin in 15 batches of P. cuspidatum determined by QAMS and external standard method was less than 5.0%,indicating that there was no significant difference between the two methods. CONCLUSIONS :UPLC fingerprint combined with QAMS method is convenient and reliable for the quality evaluation of P. cuspidatum ;the quality of P. cuspidatum produced in Chongqing and Anhui province is better.
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OBJECTIVE:To establish UPLC fingerpri nt of Ligusticum sinense ,Ligusticum jeholense and Conioselinum vaginatium,and to conduct their chemometrics analysis so as to provide reference for the identification of Rhizoma Ligustici from different origins. METHODS :UPLC method combined with Similarity Evaluation System of TCM Chromatographic Fingerprints (2012 edition) were used to establish the fingerprints of Rhizoma Ligustici from different origins. Chromatographic peak identification and similarity evaluation were carried out. Cluster analysis (CA),principal component analysis (PCA) and orthogonal partial least squares discriminant analysis (OPLS-DA)were performed to analyze Rhizoma Ligustici from different origins,and screen differential components. RESULTS :Totally 13,11,11 characteristic peaks were identified in UPLC fingerprints of L. sinense ,L. jeholense and C. vaginatium ,respectively. Similarity evaluation showed that the similarity between C. vaginatium and L. jeholense were 0.312-0.541;that between C. vaginatium and L. sinense were 0.324-0.682;that between L. sinense and L. jeholense were 0.312-0.671,indicating there was great difference among Rhizoma Ligustici from different origins. CA,PCA and OPLS-DA showed that Rhizoma Ligustici from different origins were clustered into each category respectively ; chemical components represented by peak 10,peak 13,peak 12,peak 7 and peak 6 were differential components for Rhizoma Ligustici from 3 origins. CONCLUSIONS :The study establishes UPLC fingerprint of Rhizoma Ligustici from different origins , and screens 5 differential components ,which can be used to identify Rhizoma Ligustici from different origins.
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OBJECTIVE:To compare the c hemical components differences of Inula japonica before and after honey-frying. METHODS:UPLC-MS/MS method was adopted. The determination was performed on Waters ACQUITY UPLC BEH C 18 column with mobile phase consisted of 0.1% formic acid-acetonitrile (gradient elution )at the flow rate of 0.3 mL/min. The column temperature was set at 30 ℃,and sample size was 5 µL. The electrospray ion source was scanned by positive ion mode. The first order mass spectrometry scanning range was m/z 70-1 050,the second order mass spectrometry scanning range was m/z 50-1 050, and the normalized collision energy was 40,60 eV ;mass spectrum type was the peak figure ,the flow rate of sheath gas was 35 arb,the auxiliary airflow speed was 10 arb,the spray voltage was 3.80 kV,the S-lens voltage was 50 V,the heating temperature was 350 ℃,and the capillary temperature was 350 ℃. The components were identified by Qual Browser 4.1.39.1 software, referring to the online high-resolution database mzCloud and local database OTCML of high-resolution mass spectrometry of TCM , and combined with relevant literature. The principal component analysis (PCA)and orthogonal partial least squared-discriminant analysis(OPLS-DA)of I. japonica before and after honey-fried were performed by using SIMCA 14.1 statistical software ,and variable importance projection (VIP)value greater than 1 was used as the standard to screen the differential components before and after honey-frying. RESULTS :A total of 29 common chemical components were identified from I. japonica and honey-fried I. japonica,including 5 phenolic acids as 1-caffeoylquinic acid ,chlorogenic acid and 3,5-dicaffeoylquinic acid ,12 flavonoids as quercetin,luteolin and evamectin ,as well as 12 sesquiterpene lactones as 1-O-acetylinula diester ,inula bicolor lactone B and 1-O-acetyl-6-O-isobutyryl inulin. The results of PCA showed that I. japonica and honey-fried I. japonica were located on both sides of the score diagram respectively. The results of OPLS-DA showed that the VIP values of 7 components were greater than 1,which were peak 19(britanin),peak 6(quercetagitrin),peak 1(1-caffeoylquinic acid ),peak 21(vitexicarpin),peak 20(tomentosin), peak 13(spinacetin)and peak 3(daphnetin). CONCLUSIONS :After honey-fried ,the content of chemical components of I. japonica changed and decreased to a certain extent. Britanin ,quercetagitrin,1-caffeoylquinic acid ,tomentosin,vitexicarpin, spinacetin and daphnetin may be the differential components of I. japonica and honey-fried I. japonica .