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Objective:To establish UPLC fingerprint method and 2 contents determination methods of Buddleja officinalis; To provide a reference for improving the quality control standard and evaluation of Buddleja officinalis from different habitats.Methods:UPLC method was used to establish the fingerprints of 17 batches of Buddleja officinalis. The similarity evaluation, clustering analysis, principal component analysis and orthogonal partial least squares discriminant analysis were used to compare the quality differences of Buddleja officinalis from different habitats. The contents of acteoside and linarin in Buddleja officinalis were determined.Results:There were 12 common peaks in UPLC fingerprints of Buddleja officinalis, six of which were identified as echinacoside, acteoside, cynaroside, isoacteoside, linarin, and apigenin. The fingerprint similarity of 17 batches of Buddleja officinalis was more than 0.9; Buddleja officinalis from different habitats were classified into 2 groups. Five differential markers were determined by OPLS-DA analysis. The order of significance was acteoside > peak 3 > echinacoside > isoacteoside > linarin. Edgeworthia chrysantha was identified by the method of fingerprint as counterfeit. The results of content determination showed that the content of Buddleja officinalis in Hubei and Sichuan was the high and stable.Conclusion:The method can effectively analyze the differences of Buddleja officinalis from different habitats, and provide reference for the quality control of Buddleja officinalis.
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Objectives:To discuss the feasibility of Image J in quantitative analysis on thin layer chromatography (TLC) using gallic acid in Galla Chinensis as research object.Methods:Silica gel GF 254 thin-layer plate was used with chloroform-ethyl formate-formic acid (5:5:1) as the developing solvent and the images were taken under ultraviolet light (254 nm). Polyamide film was used with 75% ethanol-glacial acetic acid (50:1) as the developing solvent and 1% ferric chloride ethanol solution as the chromogenic reagent, and the images were taken under sunlight. Images obtained from the above conditions were imported into Image J to analyze and calculate the content of gallic acid in Galla Chinensis by using external standard two-point method. High-performance liquid chromatography (HPLC) was used with a mobile phase of methanol-0.1% phosphoric acid solution (15:85) at a wavelength of 273 nm to determine the gallic acid content in Galla Chinensis. Results:The quantitation limit of gallic acid on silica gel GF 254 thin-layer plate was 0.401 6 μg, the linear range was 2.855 - 9.515 μg ( r2 = 0.996 0), and the average recovery was 105.12% ( RSD=3.48%); the quantitation limit of gallic acid on polyamide film was 0.363 4 μg, the linear range was 1.427 - 4.758 μg ( r2 = 0.991 5), and the average recovery was 103.75% ( RSD=4.60%). The HPLC method had a quantitative limit of 4.42 ng, a linear range of 0.122-0.977 μg ( r2 = 0.999 9), and a recovery rate of 98.30% ( RSD = 1.40%). The accuracy, repeatability and stability of RSD were all <5%. The gallic acid content measured using Image J showed a maximum relative error of 9.30% and a minimum of 1.62% compared to the HPLC results. Conclusions:Image J is feasible for quantitative analysis of TLC and can be used as a complementary method for quality control of Chinese materia medica.
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Objective:To establish a method for determintation of chlorogenic acid and linarin in Yejuhua granules by HPLC.Methods:We applied HPLC methods. The Kromasil 100-5 C18 column (250 mm×4.6 mm,5 μm) was used, the mobile phase was acetonitrile-0.4%H 3PO 4 solution (gradient elution), the flow rate was 1.0 ml/min, the dection wavelenghth was 334 nm and the column temperture was 32 ℃. Results:Chlorogenic acid and buddleoside had good linearity in the ranges of 0.30-1.50 μg ( r2=0.999 1) and 0.12-0.62 μg ( r2=0.999 8), respectively. The average recoveries were 99.70% and 96.67%, with RSD<2%, respectively. Conclusion:The method is simple, rapid, reliable, efficient, and can be used for determination of chlorogenic acid and buddleoside in Yejuhua Granules.
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Objective:To establish the high performance liquid chromatography (HPLC)fingerprints of Zhuanggu Guanjie Pills, which provided the basis for its quality evaluation.Methods:HPLC was used with Agilent Eclipse XDB-C 18 column (4.6 mm×250 mm, 5 μm);mobile phase was acetonitrile-0.1% acetic acid water; gradient elution; flow rate was 1 ml/min; column temperature was at 35 ℃; detection wavelength was 254 nm; injection volume was 10 μl. The HPLC fingerprints of 15 batches of Zhuanggu Guanjie Pills were established and similarity analysis was carried out, and the contents of 18 components were estimated. Results:In the fingerprint study, isopsoralen was used as the reference peak, 40 common peaks were marked and 18 peaks were identified and the similarity between the fingerprints of 15 batches of Zhuanggu Guanjie Pills and the control fingerprints was greater than 0.99.Conclusion:This method is easy to operate and has high accuracy, which can provide basis and reference for the quality evaluation of Zhuanggu Guanjie Pills.
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Objective:To establish a method for the determination of four effective components in Paeoniae Radix Alba and evaluate its quality of Paeoniae Radix Alba by principal component analysis. Methods:The effective components of Paeoniae Radix Alba were extracted by ultrasonic extraction method with ethanol. Wondasil WR C18 chromatographic column (250 mm×4.6 mm,5 μm) was used, and the mobile phase was acetonitrile-water, the flow rate was set at 1 ml/min, the column temperature was set at 30 ℃, and the total operation time was 65 min. The mass score of active components was imported into SPSS for principal component analysis. Results:The linear ranges of Paeoniflorin, Paeoniflorin, Benzoyl Paeoniflorin and Pallyl Paeoniflorin were 0.020 1-3.820 0 μg ( r2=0.999 4), 0.015 9-2.850 0 μg ( r2=0.999 2), 0.008 2- 1.820 0 μg ( r2=0.999 1), 0.003 2-0.970 0 μg ( r2=0.999 5). The quality of the 10 batches of Paeoniae Radix Alba samples from Anhui province was the best, while that from Sichuan province was the worst. Conclusions:HPLC method was established for the determination of four effective components in Paeoniae Radix Alba, and principal component analysis and evaluation of 10 batches of Paeoniae Radix Alba. Bozhou, Anhui Province, was identified as the main production area of Paeoniae Radix Alba, which can provide reference for the quality control and preparation production of Paeoniae Radix Alba.
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Objective:To establish a HPLC method for determinating 9 components simultaneously in Swertia chirayita. Methods:By useing water Sunfire C18 column (4.6 mm× 250 mm,5 μm); Gradient elution was carried out with methanol-0.05% phosphoric acid solution as mobile phase. Setting the column temperature at 30 ℃, the flow rate at 1.0 ml/min, and the detection wavelength at 254 nm.Results:9 components showed good linear relationship within the injection quality range. The recovery rates of wertiamarin, Gentiopicroside, Angelica glycosides,Mangiferin, Isolysine, Gentianoside, Diol glycoside, 8-hydroxy-1,3,5 trimethoxyketone, and Daisy leaf gentinone were 95.38%, 92.41%, 95.14%, 91.87%, 92.24%, 92.51%, 95.08%, 91.72%, 95.74% ( n=6). Conclusion:The method is simple, efficient, sensitive, accurate, economical and practical, with repeatability and stability. It could provide reference for the quality control and comprehensive utilization of Swertia chirayita.
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Objective:To establish the fingerprints of Microctis Folium by ultra high performance liquid chromatography (UPLC); To determine the contents of three flavonoids in the Microctis Folium; To evaluate the quality difference of Microctis Folium from different producing areas. Methods:The fingerprints were performed on Agilent ZORBAX SB C18 column (2.1 mm×150 mm,1.8 μm). The mobile phase was acetonitrile - 0.1 % acetic acid solution with gradient elution at a flow rate of 0.30 ml/min. The column temperature was 30 ℃ and the detection wavelength was 315 nm. The common fingerprint peaks were identified by UPLC-mass spectrometry, and the identification results were confirmed by comparison of reference materials. Waters Cortecs T3 C18 chromatographic column (2.1 mm × 100 mm,1.6 μm) was used for content determination. The mobile phase was methanol-0.1 % formic acid solution with gradient elution at a flow rate of 0.35 ml/min. The column temperature was 30 ℃ and the detection wavelength was 339 nm. The contents of vitexin, isovitexin and narcissoside in 15 batches of Microctis Folium from different habitats were determine. Results:There were 11 common peaks in the fingerprint of Microctis Folium. Identified by mass spectrometry and confirmed by reference substance,10 chemical components were identified, including caffeic acid, p-hydroxycinnamic acid, ferulic acid, vitexin, isovitexin, kaempferol-3-O-rutoside, astragaloside, narcissoside, isorhamnetin-3-O-glucoside and linden glycoside. The similarity between the fingerprints of 15 batches of Microctis Folium and the control fingerprint was greater than 0.95, indicating that the overall similarity of the fingerprints of Microctis Folium from different producing areas was high. The total contents of three active components were 3.23-5.64 mg/g in Yangjiang City, Guangdong, 3.60-5.78 mg/g in Zhanjiang City, Guangdong, 4.68-5.73 mg/g in Yulin City, Guangxi and 3.87-5.21 mg/g in Wuzhishan City, Hainan . There was no significant difference in the content of three active components in different producing areas. Conclusion:The fingerprints and the determination method established in the study are stable and feasible, which can be used for the quality evaluation of Microctis Folium.
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Objective:To establish an HPLC-DAD-ELSD method for the simultaneous determination of eight main active components in Buyang Huanwu Decoction, including hydroxysafflor yellow A, paeoniflorin, calycosin glycoside, ferulic acid, ononin, calycosin, fermononetin and astragaloside.Methods:Agilent Eclipse XDB-C18 column (250 mm×4.6 mm, 5 μm) was used with acetonitrile-0.1% formic acid as the mobile phase. The flow rate was 1.0 ml/min; the column temperature was 30 ℃; the detection wavelengths were 230 nm (paeoniflorin), 254 nm (calycosin glycoside, ononin, calycosin, fermononetin), 322 nm (ferulic acid) and 403 nm (hydroxysafflor yellow A); the drift tube temperature of the evaporative light scattering detector was 60 ℃; the carrier gas flow rate was 1.6 L/min.Results:Under these conditions, the separation of hydroxysafflor yellow A, paeoniflorin, calycosin glycoside, ferulic acid, ononin, calycosin, fermononetin and astragaloside was good, and the linear relationship was in line with the requirements ( r=0.994 0-0.999 9). The average recovery was 97.8% - 101.4% ( RSD was 1.28% - 3.70%). Conclusion:The method is simple, stable and reproducible, and can be used for the quality control of Buyang Huanwu Decoction.
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Objective:To compare the quality of Astragali Radix at different harvest time; To revise the content determination indexes of Astragali Radix in Chinese Pharmacopoeia. Methods:An Agilent Eclipse XDB-C18 column (4.6 mm × 150 mm, 5 μm) was used for the determination of saponins with acetonitrile-water solution as mobile phase in a gradient mode. The drift tube temperature of ELSD was 60 ℃; the pressure was 30 psi; the gain was 800 ℃; the flow rate was 1.0 ml/min; the column temperature was 30 ℃; the injection volume was 20 μl; the acetonitrile-0.2% formic acid solution was used as mobile phase for the determination of flavonoids in a gradient mode; the flow rate was 1.0 ml/min; the detection wavelength was 260 nm; the column temperature was 30 ℃; the 10 μl was injected. The limited range as an indicator for determining Astragali Radix content was determined by investigating the extraction method and extraction time of Astragaloside Ⅰ and detecting the content of Astragaloside Ⅰ in 12 batches of Astragali Radix from different origins. The moisture, total ash, and water-soluble extracts in Astragali Radix were determined according to the drying method, total ash determination method, and cold soaking method in the four parts of Chinese Pharmacopoeia (2020 edition), respectively. Results:The content of total saponins in Astragali Radix harvested in spring and autumn in different origins was not significantly different, but the content of total flavonoids was significantly different. Except for H11, the content of Astragaloside Ⅰ in the other batches of Astragali Radix was ≥ 0.05%, so the content limit of Astragaloside Ⅰ was proposed to be≥0.05%. The results of moisture, total ash and water-soluble extracts in the 12 batches of Astragali Radix all meet the requirements in the Chinese Pharmacopoeia. Conclusions:Astragali Radix harvested in autumn is with higher content of active components and better quality. At the same time, this study can provide a reference that the new version of Chinese Pharmacopoeia can revise the Astragaloside Ⅳ in the content determination index of Astragali Radix to Astragaloside Ⅰ .
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Objective:To comprehensively evaluate the quality of Herba Clematidis Intricatae through HPLC multi-index components, chemometrics combined with EW-TOPSIS. Methods:A total of 18 batches of Herba Clematidis Intricatae samples from seven provinces were collected. Contents of luteolin-7-O-glucoside, rutoside, hyperoside, quercitrin, quercetin, luteolin, apigenin and kaempferol in Herba Clematidis Intricatae were simultaneously determined by HPLC. Chemometrics method was used to comprehensively analyze the content determination results, and the main potential markers affecting the quality of Herba Clematidis Intricatae were analyzed. The quality of Herba Clematidis Intricatae from different origins was evaluated. Results:The eight components showed good linear relationships within their respective ranges ( r≥0.999 1), and accuracy was good ( RSD<2.0%). The chemometrics method showed that 18 batches of Herba Clematidis Intricatae could be clustered into 3 categories, showing certain regional differences. Rutoside, hyperoside and luteolin-7-O-glucoside were the indicative components affecting the difference of chemical constituents in Herba Clematidis Intricatae; results of EW-TOPSIS method showed that the optimum quality of Herba Clematidis Intricatae from Inner Mongolia and Liaoning, followed by those of Hebei, Shanxi and Shanxi, and lowest in Qinghai and Gansu. Conclusion:The established HPLC method is convenient and accurate, and combined with chemometrics and EW-TOPSIS method can be used for the comprehensive evaluation of the quality of Herba Clematidis Intricatae.
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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 investigate the changes of chemical constituents of Scutellariae Radix before and after carbonizing.Methods:Fifteen batches of Scutellariae Radix were collected. Diamonsil C18 (250 mm×4.6 mm, 5 μm) column was used; column temperature was 30 ℃; sample size was 10 μl and detection wavelength was 274 nm. The mobile phase A was 1% formic acid aqueous and B methanol, and the flow rate was 1 ml/min. The fingerprint of Scutellariae Radix before and after carbonizing was established and the changes of related components were analyzed. The content of tannin before and after processing was determined by phosphomolybdenum-tungstic acid-casein colorimetric method with gallic acid as the control.Results:Baicalin, baicalein, wogonoside and wogonin were identified by HPLC fingerprint. The contents of baicalin and wogonoside decreased, while the contents of baicalein and wogonin increased. The tannin content of Scutellariae Radix was significantly reduced after stir-frying.Conclusion:The glycosides are first converted into aglycones, then the aglycones are destroyed and the tannins are significantly reduced, which could provide a reference for the quality control of carbonized Scutellariae Radix.
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Objective:To establish UPLC fingerprint method of Buddlejae Flos standard decoction and determination method of acteoside and linarin.Methods:UPLC method was used to establish the fingerprints of 17 batches of Buddlejae Flos standard decoction. Similarity evaluation and clustering analysis were carried out on the fingerprints of Buddlejae Flos standard decoction; the chromatographic peaks of standard decoction were identified by mass spectrometry and compared with the reference materials; the contents of acteoside and linarin in Buddlejae Flos standard decoction were determined by HPLC.Results:There were 11 common peaks in the fingerprint of Buddlejae Flos standard decoction and 6 of them were identified. The similarity of the 17 batch samples was between 0.972 and 0.999. Clustering analysis classified 17 batches of Buddlejae Flos standard decoction into two categories; edgeworthia chrysantha standard decoction was identified by the method of fingerprint as counterfeit; the content determination results showed that the contents of acteoside and linarin in the standard decoction prepared from Buddlejae Flos of in Hubei and Sichuan Provinces were higher than others and were more stable.Conclusion:The method can be used to comprehensively evaluate the quality of Buddlejae Flos standard decoction and provide reference for establishing the quality standard of Buddlejae Flos dispensing granules.
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Objective:To establish a quality evaluation method for the simultaneous determination of Calycosin-7-O-β-D-Glucopyranoside and Lobetyolin in Danqi Xinmaikang boiled powders and pieces.Methods:Quantitative analysis of multi-components was performed to determine contents of Calycosin-7-O-β-D-Glucopyranoside and Lobetyolin with Calycosin-7-O-β-D-Glucopyranoside as the reference substance by single-maker (QAMS). The chromatogram conditions were established, with C18 column as solid phase, acetonitrile-water as flowing phase, 268 nm as detecting wavelength, 1.0 ml/min as flowing rate, 30 ℃ as column temperature, and 10 μl as injection volume.Results:The relative correction factor between Calycosin-7-O-β-D-Glucopyranoside and Lobetyolin was 1.14. There was no significant difference of measured values between the external standard method and QAMS ( P>0.05). With Calycosin-7-O-β-D-Glucopyranoside retention time of 1.00, the relative retention time of Lobetyolin was 1.51 and RSD was less than 5%. Conclusion:It is feasible and accurate to evaluate the quality of Danqi Xinmaikang boiled powders and pieces by QAMS.
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Objective:To establish the HPLC fingerprint of Centellae herba and determine the content of asiaticoside, madecassic acid and asiaticoside B simultaneously; To compare the quality differences of Centellae herba collected in different months. Methods:The chromatographic condition was a Shimadzu InertSustain C18 column (4.6 mm×250 mm, 5 μm) with a mobile phase consisting of acetonitrile and 2 mmol/L beta cyclodextrin in gradient elution at the flow rate of 0.8 ml/min. The detection wavelength was 204 nm, and the column temperature was 30 ℃. The different Centellae herba materials of collected in 2-12 months from Chenzhou were studied by the similarity evaluation combined with cluster analysis, principal component analysis and the three contents determination. Results:The HPLC fingerprint of Centellae herba was established and 9 common peaks were designated. The eleven samples were different, which can be aggregated into 4 categories and the quality of Centellae herba collected in July was the best. Conclusion:The established fingerprint and multi-components quantitative method are stable and reliable, which can provide a reference for the quality control and the utilization of Centellae herba resource.
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Objective:To establish a qualitative and quantitative analysis method of ginsenoside Rb1, cinnamic acid, paeoniflorin and berberine in Wenxin formula based on UPLC-MS/MS MRM model so as to provide a rapid and accurate evaluation method for the research and development of new drugs.Methods:Adopting Waters ACQUITY UPLCTM HSS T3 (2.1 mm×100 mm, 1.8 μm) and gradient elution was performed by mobile methanol-0.03% formic acid water. chromatographic column was used with electrospray ionization source in the scanning mode of multiple reactive ion monitoring (MRM) for ion separation and screening. The retention time and the relative abundance ratio (qualitative ion pairs/quantitative ion pairs) was used for qualitative analysis, while quantitative ion pairs was used for quantitative analysis.Results:The four components tested in Wenxin Formula have been qualitatively detected and showed a good linear relationship, the method showed accuracy, precision, repeatability, and stability, the recovery rate was 96.24%-104.19% and RSD was 1.29%-3.30%. Conclusion:The established method is simple, accurate, rapid and sensitive, which is reliable for the qualitative and quantitative study of the four main components in Wenxin Formula.
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Objective:To establish a method of measuring the contents of gallic acid, brevifolin, corilagin, geraniin, ellagic acid and rutin in Phyllanthus urinaria L. simultaneously with fingerprint study for analysis. Methods:Phyllanthus urinaria L. was extracted by ultrasound with 50% methanol. Chromatographic separation was performed on a Phenonmenex Luna C18 (4.6 mm×250 mm, 5 μm). The mobile phase consisted of acetonitrile (A) and 0.1% phosphoric acid aqueous solution (B) with gradient elution. The flow rate was 1.0 ml/min. The column temperature was 25 ℃, and the injection volume was 10 μl. The detection wavelength was 270 nm. HPLC fingerprints of Phyllanthus urinaria L. from different habitats was established. PCA and OPLS-DA were used to analyze the differences in chemical components of different habitats. Results:Gallic acid, brevifolin, corilagin, geraniin, ellagic acid and rutin showed good linearity at 0.042 8-0.641 6, 0.033 4-0.501 4, 0.142 2-2.133 1, 0.383 1-5.746 5, 0.063 1-0.946 2 and 0.019 2-0.287 8 μg, respectively. The average recovery rate of them was 103.65%, 96.39%, 101.85%, 95.04%, 98.79% and 98.33%, respectively. The HPLC fingerprints of different habitats contained 14 characteristic common peaks, and six compounds characteristic peaks were identified. PCA analysis showed that the chemical components of Phyllanthus urinaria L. from different habitats were different. Geraniin, ellagic acid and corilagin were screened by OPLS-DA. Conclusions:The method is efficient, accurate and sensitive, which can be used to measure the six components in Phyllanthus urinaria L.. The established HPLC fingerprint of different habitats combined with the measrurement method of six components can be used for the quality control and evaluation of Phyllanthus urinaria L..
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Objective:To study the HPLC fingerprints of Coptidis Rhizoma- Magnoliae Officmalis Cortex formula granules and the differences of active ingredients in different proportions; To explore the content changes of key components in different proportions of Coptidis Rhizoma- Magnoliae Officmalis Cortex. Methods:HPLC was used to determine the contents of several alkaloids and total phenol of Magnolia officinalis in Coptidis Rhizoma- Magnoliae Officmalis Cortex formula granules and their fingerprints, and the similarity evaluation, cluster analysis and principal component analysis were performed. Results:The similarity of fingerprint of 10 batches of Coptidis Rhizoma- Magnoliae Officmalis Cortex was > 0.950. 17 common peaks were identified, and 6 components were identified. Compared with single medicine, the contents of alkaloids and total phenols in the Coptidis Rhizoma- Magnoliae Officmalis Cortex formula granules were significantly reduced. The contents of multiple alkaloids and total phenols in the Coptidis Rhizoma- Magnoliae Officmalis Cortex formula granules in different proportions were different, and the contents of alkaloids and total phenols were the highest when the proportion of Coptidis Rhizoma- Magnoliae Officmalis Cortex was 2∶1. Conclusion:The contents of main components of Coptidis Rhizoma- Magnoliae Officmalis Cortex formula granules with different proportions are different, which can provide a certain basis for studying the compatibility mechanism of TCM couplet medicines.
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Objective:To establish an UHPLC-PDA method for determinating the content of 7 iridoid glycosides and 4 flavonoids constitutents simultaneously in Xiaoer-Ganyan granules. Methods:To take Agilent Ecilipse C18 (2.1 mm × 100 mm, 1.6 μm), and the colunm temperature was at 30 ℃. The mobile phase consists of acetonitrile (A) and 0.05% phosphoric acid (B) in gradient elution at a flow rate of 0.3 ml/min. The detection wavelength was set at 240 and 278 nm.Results:The linear ranges of swertiamain, gentiopicrin, sweroside, shanzhiside methy ester, gardenoside, genipin-1-β-D-gentiobioside, geniposide, baicalin, wogonoside, baicalein and wogonin were 19.16-306.56 μg ( r=0.999 4), 3.34-53.28 μg ( r=0.999 1), 5.30-84.64 μg ( r=0.999 5), 0.80-12.80 μg ( r=0.999 4), 0.46-7.20 μg ( r=0.999 2), 2.78-44.48 μg ( r=0.999 6), 6.02-96.16 μg ( r=0.999 9), 33.22-531.36 μg ( r=0.999 9), 3.92-62.72 μg ( r=0.999 2), 2.38-37.92 μg ( r=0.999 7), 1.32-20.96 μg ( r=0.999 9), respectively. The average recoveries ( n=9) varied from 94.62%-107.53% with RSDs no more than 3.0%. Conclusion:Method validation suggested that the developed method was suitable for simultaneous determination of 11 major constitutents in Xiaoer-Ganyan granules, thus providing reference for the improvement of quality standard of the drug.
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Objective:To compare the content change of 6 constituents in Plantaginis Semen from different habitats before and after salt processing. Methods:HPLC method was used to quantitatively analyze 6 ingredients in Plantaginis Semen and processed with salt including geniposidic acid, plantagoguanidinic acid, quercetin, kaempferol, verbascoside and isoverbascoside. Results:The geniposidic acid, plantagoguanidinic acid, quercetin, kaempferol, verbascoside and isoverbascoside were well separated. The linear ranges of which were 0.259 2-3.628 8 μg ( r=0.999 8), 0.054 3-0.760 5 μg ( r=0.999 6), 0.030 0-0.420 6 μg ( r=0.999 4), 0.055 6- 0.777 8 μg ( r=0.999 5), 0.287 0-4.018 0 μg ( r=0.999 8), 0.033 1-0.463 1 μg ( r=0.999 7), respectively. Average recovery rates were 98.68%, 98.46%, 98.87%, 98.99%, 98.34%, 98.75% ( n=6), respectively. There were mild differences in the contents of 6 ingredients of 8 batches of Plantaginis Semen from 5 different habitats. There were no obvious differences between the raw products and the products after salt process in Plantaginis Semen. The content of flavonoids, geniposidic acid and isoverbascoside in Plantaginis Semen were significantly increased after salt process, while the content of verbascoside was reduced. Conclusion:HPLC method to quantitatively analyze the 6 constituents in Plantaginis Semen before and after salt process could provided a reference for the quality change and the material basis for the efficacy of Plantaginis Semen before and after salt process.