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OBJECTIVE：To esta blish a UPLC fingerprint of Pyrrosia petiolosa from southwest China ，and to determine the contents of 4 kinds of phenolic acids （neochlorogenic acid ，caffeic acid ，chlorogenic acid and cryptochlorogenic acid ）. METHODS：The determination was performed on Waters Cortecs T 3 C18 column（100 mm×2.1 mm，1.6 μm）with mobile phase consisted of methanol- 0.1％ phosphoric acid （gradient elution ）at the flow rate of 0.35 mL/min. The detection wavelength was set at 326 nm. The column temperature was 30 ℃，and injection volume was 1 μL. UPLC method was used to establish the UPLC fingerprint of P. petiolosa in combination with the Similarity Evaluation System of TCM Chromatographic Fingerprints （2012 edition）. Cluster analysis and principle component analysis （PCA）were performed by using SPSS 20.0 software. The contents of 4 kinds of phenolic acids in 20 batches of P. petiolosa were determined by external standard method. RESULTS ：There were 9 common peaks for the UPLC fingerprint of P. petiolosa . Peaks 1，3，4，5 and 9 were identified as neochlorogenic acid ，caffeic acid，chlorogenic acid ，cryptochlorogenic acid and isochlorogenic acid C ，respectively. RSDs of the relative retention time of each peak in different batches of P. petiolosa were 0-0.68％，and the RSDs of the relative peak area were 0-62.35％. The similarities between the fingerprint of 20 batches of medicinal materials and the control chromatogram were not less than 0.990. The result of cluster analysis showed that P. petiolosa from different regions could be sorted into three species. Results of PCA showed the differences among P. petiolosa from different regions. The linear range of neochlorogenic acid ，caffeic acid ，chlorogenic acid and cryptochlorogenic acid were 0.61-61.41，0.18-17.60，2.00-200.11，0.62-61.51 μ g/mL （R2＞0.999 9）. RSDs of precision ， reproducibility and stability tests were all lower than 2.00％. The recoveries were 96.23％-98.17％（RSD＝0.96％-2.28％， n＝6）. Among 20 batches of samples ，the contents of above 4 kinds of phenolic acids were 0.385 3-1.891 9，0.018 0-0.129 5，2.569 5-10.676 0，0.563.5-1.860 5 mg/g. CONCLUSIONS ： The established UPL C fingerprint could reflect the main chemical constituents of P. pedunculata . Phenolic acids could be used as the main evaluation indexes for the quality of P. petiolosa . The quality order of P. petiolosa from southwest China was Chongqing product＞Sichuan product ＞Guizhou product.
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Objective: To investigate the effects of neochlorogenic acid, chlorogenic acid, cryptochlorogenic acid, isochlorogenic acid B, isochlorogenic acid A, and isochlorogenic acid C in effective parts of rhizoma arthritis against rhizoma arthritis from different sources of Miao medicine Periploca forrestii Schltr. The determination of 6 kinds of caffeoacylquinic acid chemical components and comprehensive analysis of their quality combined with chemometrics provide a basis for a reasonable and effective evaluation of the efficacy of Miao Medicine Periploca forrestii Schltr against rheumatoid arthritis. Methods: Simultaneous determination was performed by HPLC-UV method. The column was Xtimate C18 (250 mm×4.6 mm, 5 μm), the mobile phase was 0.1% formic acid-acetonitrile, gradient elution, the injection volume was 10 μL, and the flow rate was 1 mL/min. The column temperature is 25 ℃ and the detection wavelength is 327 nm. SPSS24.0 and SIMCA14.1 software are used for comprehensive analysis and evaluation of the quality of medicinal materials. Results: The content of 21 batches of Periploca forrestii Schltr samples from different sources was determined. Through the cluster analysis, the 21 batches of samples were classified into type III, of which the quality of types II and III was better; principal component analysis and partial least squares discriminant analysis The results were consistent with the clustering results. The chlorogenic acid and isochlorogenic acid C were screened to be the markers that caused the differences in the quality of Periploca forrestii Schltr from different sources. Conclusion The determination of the contents of six caffeoacylquinic acid components combined with stoichiometry can further evaluate the efficacy and quality of the anti-rheumatoid arthritis effect of Periploca forrestii Schltr, and provide a reference basis for the quality control of Periploca forrestii Schltr.
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Objective: To establish a rational method for Laportea bulbifera quality control. Methods: The fingerprint technique and multi-component quantitation were used to study the quality control of L. bulbifera by UHPLC. The 12 batches of L. bulbifera UHPLC fingerprint were evaluated by the evaluation system on similitude degree of chromatogram fingerprint of traditional Chinese medicine. Results: The quality control methods of Miao medicine L. bulbifera for simultaneous determination of 10 components (including neochlorogenic acid, cryptochlorogenic acid, chlorogenic acid, rutin, isoquercitrin, luteoloside, kaempferol-3-O-rutinoside, quercitrin, epigallocatechin and epicatechin) were established. The linear, precision, repeatability and stability are good. The standard recoveries were 95.89%-98.62%, with RSD less than 3%. The common mode of fingerprint was established after determination fingerprints of 12 batches of samples of L. bulbifera by UHPLC. There were 20 common peaks in these samples. The similarity of the 12 batches fingerprints were in the range from 0.805 to 0.931. Conclusion: The fingerprinting and multi-index content determination methods for quantitative control of Miao medicine L. bulbifera have high sensitivity, good accuracy, stability and reliability, which can provide a theoretical and experimental foundation for quantitative control of Miao medicine L. bulbifera.
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Objective: To establish HPLC fingerprint of Eriobotryae Folium standard decoction and compare quality difference between raw and honey processed Eriobotryae Folium standard decoction, which can provide a reference for its quality control. Methods: An HPLC-DAD method was utilized. The mobile phase was acetonitrile-0.4% phosphoric acid setting for gradient elution. The HPLC fingerprints of 20 batches of standard decoction of raw and honey processed Eriobotryae Folium were established. The contents of neochlorogenic acid, chlorogenic acid, and cryptochlorogenic acid were determined simultaneously. Similarity and cluster analysis were chosen to evaluate the quality of standard decoction of raw and honey processed Eriobotryae Folium. Results: Both of the fingerprint and the contents of three kinds of chlorogenic acids of Eriobotryae Folium standard decoction had significant difference before and after the Eriobotryae Folium being processed by honey. Two chromatographic peaks were increased newly in honey processed Eriobotryae Folium. The No.1 peak refers to component of 5-hydroxymethylfurfural. The average contents of neochlorogenic acid, chlorogenic acid and cryptochlorogenic acid in raw Eriobotryae Folium standard decoction were 4.300, 4.306, and 5.432 mg/g respectively. The result of contents showed a significantly decrease in honey processed Eriobotryae Folium standard decoction. Their contents were 3.295, 3.460, and 4.118 mg/g respectively. The reduction rate of them were 23.29%, 19.06%, and 23.92% respectively. Conclusion: The method is concise and durable. It could not only be utilized to evaluate the quality of standard decoction of Eriobotryae Folium before and after processed by honey, but also to identify the quality differences of them. The study could be used for quality control of standard decoction of raw and honey processed Eriobotryae Folium, identify the quality difference of them and also provide a reference for quality control of their preparations.
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Objective: To establish a method for the determination of seven organic acids, one flavone and two iridoid terpenoids in Lonicerae Japonicae Flos from different habitats. Methods: The content of 10 components in Lonicerae Japonicae Flos from different habitats were determined by ultra-performance liquid chromatography (UPLC). The mobile phase for gradient elution was 0.1% phosphoric acid solution (A)- methanol (B); The flow rate was 0.3 mL/min, and the column temperature was 30 ℃. Results: A UPLC method for simultaneous determination of seven organic acids, one flavone and two iridoid terpenoids in Lonicerae Japonicae Flos was established. Principal component analysis (PCA) and partial least squares method (PLS-DA) were used to analyze the distribution and characteristics of 10 constituents of Lonicerae Japonicae Flos collected from different habitats; Three production areas of Shandong, Jiangsu and Shaanxi are respectively grouped into one group. Conclusion: The method is stable and feasible, which could be used as a reference for evaluating the quality of Lonicerae Japonicae Flos in a more comprehensive way.
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Objective: To study the quality control method of Miao medicine Inula cappa based on anti-inflammatory active ingredients. Methods: Firstly, a representative and characteristic chemical composition of effective components in I. cappa was established as an indicator component for multi-index quantitative fingerprinting. Then, the quality of I. cappa in different areas of Guizhou Province was evaluated by quantitative analysis of multiple indicators and fingerprint analysis. Results: The HPLC fingerprints and multi-index content determination methods of 35 batches of I. cappa were established. Eight of 17 common peaks of the liquid chromatographic fingerprints of I. cappa were identified. The results showed that the similarity was 0.898-0.997, eight components of which were used as indicators to determine the content of chlorogenic acid, neochlorogenic acid, cryptochlorogenic acid, isochlorogenic acid B, isochlorogenic acid A, isochlorogenic acid C, cynarin and luteolin, which were 0.353-3.765, 0.056-0.495, 0.086-0.526, 0.306-2.526, 0.861-7.353, 0.729-4.268, 0.052-0.424, 0.148-1.102 mg/g, respectively. Conclusion: The fingerprinting and multi-index content determination methods based on anti-inflammatory active ingredients established have high sensitivity, good accuracy, stability and reliability, which can be used for quantitative control of Miao medicine I. cappa.
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Objective: To establish HPLC coupled with wavelength switching and gradient elution method (HPLC-DVD) for simultaneous determination of 14 active components (neochlorogenic acid, chlorogenic acid, cryptochlorogenic acid, geniposide, 4-hydroxyacetophenone, scutellarin, isochlorogenic acid B, isochlorogenic acid A, isochlorogenic acid C, oroxylin A 7-O-glucuronide, wogonoside, baicalein, wogonin and oroxylin A and one auxiliary material (benzoic acid) in Yinzhihuang Oral Solution (YOS). Methods: The chromatographic separation was achieved on Welch Ultimate XB-C18 (250 mm × 4.6 mm, 5 μm) column with acetonitrile-0.1% phosphoric acid solution as mobile phases for gradient elution, at the flow rate of 0.8 mL/min in the first 30 min and 1.0 mL/min in the follow-up; The detection wavelength was set at 325 nm for neochlorogenic acid, chlorogenic acid and cryptochlorogenic acid, 238 nm for geniposide, 275 nm for 4-hydroxyacetophenone, 228 nm for benzoic acid, 325 nm for scutellarin, isochlorogenic acid B, isochlorogenic acid A and isochlorogenic acid C, 203 nm for oroxylin A 7-O-glucuronide and wogonoside, and 274 nm for baicalein, wogonin and oroxylin A. The volume of sample injection was 10 μL. Results: The fifteen active components were well separated and showed good linearity, such as neochlorogenic acid 74.46-1 574.42 ng (r = 0.999 8), chlorogenic acid 34.58-741.1 ng (r = 0.999 6), cryptochlorogenic acid 34.65-742.62 ng (r = 0.999 7), geniposide 234.42-5 024.45 ng (r = 0.999 9), 4-hydroxyacetophenone 74.46-1 574.42 ng (r = 0.999 9), benzoic acid 321.79-6 897.1 ng (r = 0.999 8), scutellarin 44.7-958.08 ng (r = 0.999 7), isochlorogenic acid B 32.53-697.22 ng (r = 0.999 5), isochlorogenic acid A 8.6-184.38 ng (r = 0.999 6), isochlorogenic acid C 31.93-684.3 ng (r = 0.999 7), Oroxylin A 7-O-glucuronide 254.82-5 461.66 ng (r = 0.999 5), wogonoside 10.18-218.12 ng (r = 0.999 9), baicalein 92.81-1 989.33 ng (r = 0.999 6), wogonin 31.17-668 ng (r = 0.999 5), and oroxylin A 11.74-251.73 ng (r = 0.999 8). The precision was good, and RSD was not more than 0.75%. The repeatability was good, and the RSD was not more than 1.95%. The stability was good in 8 h, and RSD was not more than 1.77%. The average recoveries and corresponding RSD values were 100.69% (0.55%), 101.99% (1.78%), 99.20% (0.72%), 100.13% (0.48%), 100.96% (1.74%), 100.02% (0.46%), 101.14% (0.27%), 99.87% (0.59%), 100.21% (1.56%), 102.18% (0.33%), 99.00% (1.02%), 98.82% (0.65%), 98.31% (0.58%), 96.01% (0.44%), and 100.56 (0.71%), respectively. The content of 10 batches of neochlorogenic acid, chlorogenic acid, cryptochlorogenic acid, geniposide, 4-hydroxyacetophenone, benzoic acid, scutellarin, isochlorogenic acid B, isochlorogenic acid A, isochlorogenic acid C, oroxylin A 7-O-glucuronide, wogonoside, baicalein, wogonin and oroxylin A were 0.246-0.322, 0.213-0.290, 0.203-0.267, 1.786-2.047, 0.035-0.046, 2.393-2.541, 0.263-0.392, 0.139-0.216, 0.032-0.067, 0.208-0.250, 2.120-2.648, 0.063-0.102, 0.081-1.429, 0.164-0.246, and 0.079-0.110 mg/mL. Conclusion: HPLC coupled with wavelength switching and gradient elution method has been established for simultaneous determination of 15 components in YOS. The method is simple, quick, accurate, and it can be used for content determination and quality control of YOS.
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Objective: To study Lonicerae Japonicae Flos, Lonicerae Japonicae Caulis, and Lonicerae Japonicae Leaves by UPLC method, and study the different parts of Lonicera japonica by the fingerprint similarity evaluation, cluster analysis, principal component analysis, and other chemical pattern recognition technologies, in order to provide scientific basis for the comprehensive utilization of L. japonica. Methods: The method was carried out on an ACQUITY UPLC BEH C18 column (100 mm × 2.1 mm, 1.7 μm) by a gradient elution using acetonitrile and 0.1% phosphoric acid. The flow rate was 0.3 mL/min, The column temperature was 30 ℃. The sample room temperature was 8 ℃. The detection wavelengths were 326, 238, and 250 nm, and the injection volume was 1 μL. Results: The UPLC fingerprint of 28 batches of samples from different parts of Lonicerae Japonicae were set up and 14 common peaks were obtained. They were new chlorogenic acid, chlorogenic acid, cryptochlorogenic acid, caffeic acid, loganin, rutinum, luteoloside, isochlorogenic acid B, isochlorogenic acid A and isochlorogenic acid C. There were some differences in chemical composition and quantity of Lonicerae Japonicae Flos, Lonicerae Japonicae leaves, and Lonicerae Japonicae Caulis. PCA and cluster analysis revealed the similarity and difference of 28 batches of samples from different parts of L. japonica. Conclusion: The combination of clustering analysis and principle component analysis could be used to confirm that the chemical constituents of Lonicerae Japonicae Flos and Lonicerae Japonicae leaves were similar, but there was a difference between Lonicerae Japonicae Flos and Lonicerae Japonicae Caulis. The established fingerprint method can provide a reference for the quality control of Lonicerae Japonicae Flos, Lonicerae Japonicae leaves, and Lonicerae Japonicae Caulis.
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Objective: To establish an HPLC method for simultaneous determination of geniposide,chlorogenic acid,neochlorogenic acid,cryptochlorogenic acid,isochlorogenic acid A,B and C in Qinggan Lidan mixture,in order to provide references for its quality control. Method: The analysis of methanol extract of this drug was performed on a 35℃ Luna C18 column (4.6 mm×250 mm,5μm),with the mobile phase comprised of acetonitrile-0.4% phosphoric acid flowing at 1.0 mL·min-1 in a gradient elution mode (0-10 min,8%-12%A;10-30 min,12%A;30-60 min,12%-35%A),and the detection wavelengths were set at 238 and 327 nm. Result:Geniposide,chlorogenic acid,neochlorogenic acid,cryptochlorogenic acid,isochlorogenic acid A,B and C were completely separated,and well separated from other constituents. The linear ranges of geniposide,chlorogenic acid,neochlorogenic acid,cryptochlorogenic acid,isochlorogenic acid A,B and C were 0.188-2.355,0.083-1.040,0.074-0.920,0.075-0.940,0.064-0.800,0.076-0.955,0.071-0.888 μg (r ≥ 0.999 0),respectively. The average recoveries were 99.45%,98.45%,99.06%,98.50%,98.16%,101.01%,96.93%,with the RSDs of 0.5%,1.8%,1.3%,2.4%,2.3%,1.6%,1.6%,respectively.The contents of geniposide,chlorogenic acid,neochlorogenic acid,cryptochlorogenic acid,isochlorogenic acid A,B and C were 3.420-3.794,0.835-0.890,1.222-1.275,1.064-1.210,0.377-0.398,0.419-0.464 and 0.362-0.405 g·L-1,respectively. Conclusion:This method can be used for simultaneous determination of muti-ingredients in Qinggan Lidan mixture,and the established method is simple and accurate,with a good reproducibility and high sensitivity. It can be used for the quality control of Qinggan Lidan mixture.
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Objective: To establish an HPLC method to simultaneously determine 10 active ingredients in Yinzhihuang Oral Liquid (YOL) and provide scientific basis for the quality control, evaluation and standard revision of Yinzhihuang preparations. Methods: An HPLC-UV method was used with a Dikma Diamonsil C18 column (200 mm × 4.6 mm, 5 μm). The mobile phase was acetonitrile-0.1% acetic acid solution with gradient elution (0-15 min, 8%-12% acetonitrile; 15-40 min, 12%-30% acetonitrile; 40-55 min, 30%-60% acetonitrile; 55-75 min, 60%-35% acetonitrile; 75-80 min, 35%-8% acetonitrile). The detection wavelength was 240 nm. The flow rate was 1.0 mL/min. The column temperature was 30 ℃. The injection volume was 20 μL. Results: Ten active ingredients (neochlorogenic acid, chlorogenic acid, cryptochlorogenic acid, geniposide, p-hydroxyphenylacetone, scutellarin, baicalin, quercetin, baicalein and wogonin) in YOL were simultaneously determined. The linearity was good (r ≥ 0. 999 0), the limit of detection and quantification were 0.003-0.018 μg/mL and 0.009-0.055 μg/mL. The average recoveries were 99.7%-102.6% with RSDs of 0.34%-6.14%. The average content of the above 10 ingredients was in turn (0.21 ± 0.09), (0.47 ± 0.01), (0.87 ± 0.06), (4.71 ± 0.27), (0.94 ± 0.20), (4.52 ± 0.80), (41.75 ± 3.53), (9.85 ± 1.67), (0.45 ± 0.09), (3.51 ± 0.89) mg/mL. The content of baicalin and geniposide was 35.44-45.82 mg/mL and 4.16-4.92 mg/mL in eight batches, respectively. All eight batches of YOL meet the requirements of the Chinese Pharmacopoeia 2015 with qualified in quality. Conclusion: The established HPLC method is simple, specific, sensitive, stable, precise, accurate, and reproducible, which can be used for quality control and evaluation of YOL.
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Objective: To optimize the processing technology of stir-fried Euodiae Fructus with the water decoction of Coptidis Rhizoma by L9(34) orthogonal design. Methods: The factors including the dosage of Coptidis Rhizoma, stir-frying temperature and stir-frying time, and phenolic acids (neochlorogenic acid, chlorogenic acid, caffeic acid, and cryptochlorogenic acid), flavonoids (rutin, hyperin, and narcissoside), alkaloids (dehydroevodiamine, evodiamine, rutaecarpine, evocarpine, and dihydroevocarpine), and volatile oils in Euodiae Fructus were taken as evaluation indexes to optimize the processing technology. Results: The best processing technology for stir-fried Euodiae Fructus with the water decoction of Coptidis Rhizoma was as follows: the dosage ratio of Euodiae Fructus to Coptidis Rhizoma 10:1, stir-frying temperature 150 ℃, and stir-frying time 8 min. Conclusion: Simultaneously, taking the content of four kinds of components as the indexes, the method for optimizing the optimal processing technology of stir-fried Euodiae Fructus with the water decoction of Coptidis Rhizoma is stable, reliable and feasible.
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Objective: To establish HPLC fingerprint of antipyretic lotion for children and determine the content of 10 components (neochlorogenic acid, chlorogenic acid, cryptochlorogenic acid, caffeic acid, forsythiae A, isochlorogenic acid B, isochlorogenic acid A, isochlorogenic acid C, rosmarinic acid and forsythin). Methods: The analysis of antipyretic lotion for children was performed on the Kromasil 100-5 C18 (250 mm × 4.6 mm, 5 μm) chromatographic column, with mobile phase comprising of 0.1% phosphate acid-acetonitrile flowing at 1 mL/min in a gradient elution manner, and the column temperature was 35 ℃, and detection wavelength was set at 330 nm. With forsythia A as reference peak, HPLC fingerprint of 11 batches of preparations was established; Based on the conditions of fingerprint chromatogram, the content of 10 components was determined at the detection wavelength of 330 and 280 nm and the multi-index content of 11 batches of the preparation was determined. Results: HPLC fingerprint was established, a total of 37 peaks were selected as the common peaks, of which 22 peaks were identified, and the similarities of 11 batches of preparations were between 0.987 and 0.999. The linear relationships of neochlorogenic acid, chlorogenic acid, cryptochlorogenic acid, caffeic acid, forsythiae A, isochlorogenic acid B, isochlorogenic acid A, isochlorogenic acid C, rosmarinic acid, and forsythioside were good in the range of 14.18-141.78, 20.53-205.63, 14.38-143.78, 5.62-56.19, 22.22-222.22, 8.40-83.98, 5.70-57.02, 7.46-76.36, 16.95-169.48, 8.59-85.94 g/mL, respectively. The average recoveries were 109.51%, 98.73%, 99.41%, 90.63%, 92.73%, 95.39%, 91.87%, 106.50%, 95.23%, and 108.71%. The content of neochlorogenic acid, chlorogenic acid, cryptochlorogenic acid, caffeic acid, forsythiae A, isochlorogenic acid B, isochlorogenic acid A, isochlorogenic acid C, rosmarinic acid, and forsythin in the 11 batches were in the range of 306.38-457.85, 607.67-854.71, 306.81-469.02, 95.65-170.64, 484.41-819.44, 234.28-322.01, 145.42-226.85, 219.11-292.21, 347.94-507.74, 201.35-261.94 mg/mL, respectively. Conclusion: The method is accurate, simple, stable and reliable, which can be used for the quality control of antipyretic lotion for children.
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Objective: To establish a rapid, accurate, and practical HPLC method for simultaneous determination the content in Qiju Dihuang Oral Liquid (QDOL) of 5-HMF, morroniside, chlorogenic acid, cryptochlorogenic acid, loganin, paeoniflorin, verbascoside, luteoloside, isochlorogenic acid B, isochlorogenic acid A, isochlorogenic acid C, and paeonol. Methods: YMC ODS column (250 mm × 4.6 mm, 5 μm) was used, column temperature was set at 35 ℃, gradient elution with 0.1% formic acid aqueous solution- acetonitrile was used as mobile phase, flow rate was 1.0 mL/min, detection wavelength was 254 and 325 nm. The injection volume was 10 μL. Results: The injection amount of 5-HMF, morroniside, chlorogenic acid, cryptochlorogenic acid, loganin, paeoniflorin, verbascoside, luteoloside, isochlorogenic acid B, isochlorogenic acid A, isochlorogenic acid C, paeonol injection quality at 0.08—1.60, 0.12—2.40, 0.09—1.80, 0.06—1.20, 0.10—2.00, 0.30—6.00, 0.01—0.20, 0.01—0.20, 0.01—0.20, 0.005—0.10, 0.005—0.10, and 0.01—0.20 μg showed a good linear relationship with peak area, with good precision, repeatability and stability. The recovery rates of the samples were between 96% and 103%, the RSD was 2.13%, 3.45%, 2.86%, 2.59%, 3.15%, 3.49%, 2.19%, 3.25%, 2.37%, 2.53%, 2.91%, and 3.35%, respectively. The content of each component of the five batches of samples was stable, and the mass concentrations range of the 12 components tested were 98.56—102.56, 204.28—212.10, 18.53—18.89, 1.95—2.05, 12.31—12.54, 87.01—87.12, 5.35—5.43, 16.08—16.15, 8.69—8.72, 8.89—8.95, 5.12—5.19, and 1.87—1.94 μg/mL. Conclusion: The method simltaneosly determines the content of 5-HMF, morroniside, chlorogenic acid, cryptochlorogenic acid, loganin, paeoniflorin, verbascoside, luteoloside, isochlorogenic acid B, isochlorogenic acid A, isochlorogenic acid C, and paeonol in QDOL, which is suitable for the quality control of QDOL.
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Objective To establish a quantitative analysis method of multiple active components liquiritin, vitexin, baicalin, rutin, cryptochlorogenic acid, chlorogenic acid, quercetin, and kaempferol in Qingreling Granules (QG) based on UHPLC-ESI-HRMSn, in order to provide a comprehensive evaluation for the quality control of QG. Methods The chromatographic separation was carried on BEH C18 (100 mm × 2.1 mm, 1.7 μm) column with methanol-0.1% formic acid water as mobile phase at the flow rate of 0.3 mL/min. Full scan mode with an electrospray ionization (ESI) source was used for the detection. The quantitative determination results were calculated by the pattern recognition function of the software SIMCA 14.1 to evaluate the quality of QG. Results Liquiritin, baicalin, rutin, vitexin, quercetin, chlorogenic acid, cryptochlorogenic acid, and kaempferol all showed good liners relationship (r ≥ 0.999 0) in the ranges of 570-9 127, 10 032-160 500, 293-4 690, 1 625-26 000, 40.5-645, 41-1 325, 44-1 413, and 13-209 ng/mL, respectively. The precision, repeatability, and stability were all up to the standards. The recoveries of standard addition was 98.83% to 100.65% with precision of below 3% RSD (n = 5). The average mass fractions of liquiritin, baicalin, rutin, vitexin, quercetin, chlorogenic acid, cryptochlorogenic acid, and kaempferol in five batches of QG were 202.07-438.15, 10 258.03-11 046.56, 56.09-87.7, 689.19-818.56, 4.95-6.0, 8.87-18.37, 22.49-42.12, 3.21-4.11 μg/g, respectively. The data analyzed by SIMCA 14.1 showed that the quality deviation of five batches of QG were within ± 2. Conclusion The method established in this study is simple, rapid, sensitive and accurate. The results of methodology conform to the relevant requirements and the method can be used as a quantitative method for the active ingredients in QG. The research also provides a new basis for the quality control at the same time.
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Objective To establish the multi-wavelength fusion HPLC fingerprints of Gardeniae Fructus and to make quantitative analysis of the common peaks by ESI-Q-TOF MS. Methods The Kromasil 100-5 C18 column was used with a mobile phase of acetonitrile-0.1% phosphoric acid in gradient elution; The flow rate was 1.0 mL/min; The column temperature was 35 ℃; The detection wavelength was 238, 327, and 440 nm. Matlab7.1 was adopted for multi-wavelength fusion of the data in CSV format. Results Twenty chemical constituents were detected in fusion fingerprint, which included more information. Sixteen chemical constituents were compared with reference standards and identified by MS. The similarity of 10 batches of Gardeniae Fructus was over 0.90. Conclusion The systematic quantified fingerprint method based on the technique of multi-wavelength fusion fingerprint and identifying 16 constituents can be used for the fully quality control of Gardeniae Fructus.
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Objective: To provide references for quality evaluation of Lonicerea Japonicae Flos (LJF) through exploring correlation between color and contents of active ingredients of LJF in different development periods. Methods: The colorimeter was used to measure the color of LJF in different development periods; HPLC was applied to determine the contents of phenolic acids, flavonoids and iridoids. SPSS 17.0 software was used to analyze the correlation between color and chemical composition of LJF. Results: With the development of flower buds, the contents of phenolic acids, flavonoids compounds achieved the highest in two white stages and the contents of iridoids came to the highest in big white stage and silver flower stage. Therefore, only taking the consideration of the content of active ingredient, the best harvest time of LJF might be the big white stage. There was a significant positive correlation among contents of phenolic acids, flavonoids and brightness (L*) of LJF in different development periods, and there was a very significant negative correlation among contents of phenolic acids, flavonoids, iridoids, and browning index (BI). Conclusion: The color of LJF is closely related to the content of active ingredients, L* and BI can better link appearance and inner quality of LJF.
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Objective To evaluate the probability and quality consistence of Lonicera japonica Flos extraction and concentration intermediate by introducing and applying process performance index (PPI) PPK. Methods With the historical quality analysis date of intermediate of Lonicerae Japonicae Flos extraction and concentration process of Reduning Injection., the confidence intervals of PPK were estimated based on the Bootstrap sampling methods. Results The PPK of neochlorogenic acid, chlorogenic acid, cryptochlorogenic acid, caffeoylquinic acid, solid holdup was 1.115 6, 1.111 2, 1.117 9, 1.110 9, and 1.560 0 respectively. The PPK of solid holdup is the highest, the PPK of several phenolic acids is lower, but all the PPK can meet the production requirements, showed that the probability and quality consistence of this process is good. The lower limit of 95% confidence intervals of quality indexes was 1.068 3, 1.049 6, 1.066 7, 1.052 1, and 1.495 0 respectively, all greater than 1.000 0, indicating the results were credible. Conclusion The method can be used to evaluate the probability and quality consistence of Lonicerae Japonicae Flos extraction and concentration process, and it provides fundamental evidence on establishing quality standards for releasing or process parameters for releasing.
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Objective: To develop an UPLC method for simultaneous determination the contents of 10 active constituents [neochlorogenic acid (NCA), chlorogenic acid (CA), cryptochlorogenic acid (CCA), isochlorogenic acid A (ICAA), isochlorogenic acid B (ICAB), isochlorogenic acid C (ICAC); bacicalin, wogonoside, baicalein, and wogonin] in Yinhuang preparations. Methods: Analysis was performed on an Acquiyt UPLC BEH C18 chromatographic column (100 mm × 2.1 mm, 1.7 μm) eluted with acetonitrile- 0.4% phosphoric acid, gradient elution, and the flow rate was 0.4 mL/min, the detection wavelength was set at 326 nm, the column temperature was 40℃, and the injection volume was 1.0 μL. Results: All calibration curves were linear (r ≥ 0.999 6) over the tested ranges. The average recoveries (n = 9) ranged from 97.43% to 99.94% with RSD value below 2.0%. The contents of 11 batches of NCA, CA, CCA, ICAA, ICAB, ICAC, bacicalin, wogonoside, baicalein, and wogonin were 0.236-3.419, 5.279-26.220, 0.495-4.714, 0.130-2.702, 0.310-3.210, 0.363-5.036, 35.209-133.289, 1.493-6.635, 1.546-5.393, and 0.254-0.823 mg/g. Conclusion: This method is rapid, simple, sensitive, accurate, and reproducible, which can be used for quality control of Yinhuang preparation, and provide a reference for the formulation of quality standards to enhance in the future.
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Objective: To establish an HPLC fingerprint chromatography and determine seven compounds of multi-components in Shuangyu Granules (SG). Methods: The Kromasil C18 (250 mm × 4.6 mm, 3.5 μm) column was used with a mobile phase of acetonitrile-0.05% trifluoroacetic acid gradient elution. The flow rate was 0.8 mL/min, the column temperature was 30℃, and the detection wavelengths were 230 and 327 nm. The common peaks were identified by Q-TOF/MS. Results: The fingerprint chromatography included 17 mutual peaks, and the similarity was more than 0.95. Fourteen common peaks had been identified by LC-Q-TOF/MS, seven of which were unequivocally identified via comparing the retention times and mass spectra data with those of the standard compounds. Then the seven marker components were quantified. The developed quantitative method was validated in terms of accuracy (the recoveries ranged from 97.8% to 101.8% with RSDs less than 2%). Conclusion: The method is rapid, simple, and accurate and can be used for the quality control of SG.
ABSTRACT
Objective:To study the application of statistical process control technology to establish the real-time release criteria of alcohol precipitation process of ArtemisiaeAnnuae Herba and Lonicerae Flos. Methods: Twenty-ninebatches of samples came from alcohol precipitation process of ArtemisiaeAnnuae Herba and Lonicerae Flos were collected as the calibration set. The contents of neochlorogenic acid, chlorogenic acid, cryptochlorogenic acid, and solid content were determined to establish the quantitative real-timerelease criteria based on statistical process control technology. Thirteenbatches of alcohol precipitation process of ArtemisiaeAnnuae Herba and Lonicerae Flos were prepared under the different process conditions by the central composite design. They were regarded as the validation set to test the dependability of the real-time release criteria. Results: The established quantitative release ranges were neochlorogenic acid 0.279-0.541 mg/g, chlorogenic acid 1.941-2.610 mg/g, cryptochlorogenic acid 0.453-0.570 mg/g, and solid content3.565%-4.925%. The four index component contentsof the samples 1, 4, 8, 9, and 10 from the validation set werewithin the range of the real-time release criteria. Conclusion: Univariate statistical process control could be well monitored and understood of production process for Chinses materiamedica.They are used to achieve the purpose of real-time release.