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Objective: To establish a method for the simultaneous content determination of 14 chemical components such as D- amygdalin, puerarin, hesperidin in Fenghan Ganmao Granules (FGG) by UHPLC-UV wavelength switching method, and chemometric analysis was used to analyze the quality differences. Methods: Separation was performed on an Agilent Poroshell 120 EC-C18 (150 mm × 2.1 mm, 2.7 μm) with a gradient elution of acetonitrile and 0.1% phosphoric acid. The content of 14 chemical components in 68 batches of samples from five manufacturers was determined by switching wavelength (210, 254, 310 nm). The radar chart, similarity evaluation, heat map and hierarchical clustering analysis, and principal component analysis (PCA) were used for data analysis. Results: The content of each component was as follows, D-amygdalin 0.063-3.885 mg/g, 3'-hydroxy puerarin 0.012-1.540 mg/g, puerarin 0.036-4.017 mg/g, 3'-methoxy puerarin 0.016-1.837 mg/g, puerarin-6″-O-xyloside 0.004-0.449 mg/g, mirificin 0.021-2.076 mg/g, daidzin 0.010-1.527 mg/g, prim-O-glucosylcimifugin 0.007-0.471 mg/g, 5-O-methylvisammioside 0.062-1.029 mg/g, hesperidin 0.210-8.453 mg/g, rosmarinic acid 0.001-0.237 mg/g, oxypeucedanin hydrate 0.007-0.204 mg/g, glycyrrhizic acid 0.056-1.311 mg/g, oxypeucedanin 0.002-0.042 mg/g, respectively. Chemometric analysis showed that there were some differences among the samples from different manufacturers, and the samples from the same manufacturer were more consistent. Conclusion: The method is simple, reproducible, and specific, which provides a reference method for the overall quality evaluation of FGG.
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Objective: A new table of standards of commodity classes of Saposhnikovia Radix is formed through literature market and local area survey. To explore the scientific nature and practicability of new standards of commodity classes of Saposhnikovia Radix, according to the appearance and index components related to quality of Saposhnikovia Radix, through statistical analysis and comparison of characteristic spectrum. Methods: Samples of different specifications and grades were collected from Northeast China, Inner Mongolia, Hebei, and the other main production areas, mainstream medicine market. Measuring samples appearance, extractum, characteristic spectrum of four chromones and analyzing data and discussing the relationship between standards of commodity classes and the appearance and index components to provide datas and theoretical support for the new table. Results: According to appearance character, the standards of commodity classes of Saposhnikovia Radix divided into three specifications of wild, imitates wild, cultivated were science based. At the same time, it is suggested to increase the content of the cimifugin as the index to distinguish between wild and cultivated Saposhnikovia Radix. Conclusion: There were significant differences in appearance and index components between different standards of Saposhnikovia Radix. Whether different classes of Saposhnikovia Radix only depend on size remains to be discussed.
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OBJECTIVE: To establish the method for simultaneous determination of pim-O-glucosylcimifugin, liquiritin, 5-0-methylvisammioside and amonium glycyrrhizinate in Xinyi byan pills.METHODS: HPLC-switching wavelength method was used for content determination of 52 batches of Xinyi byan pills sample from enterprises A, B, C. The determination was performed on Kromasil C18 column with mobile phase consisted of acetonitrile-0. 1 ％ phosphoric acid at the flow rate of 1. 0 mL/min. The detection wavelengths were set at 220 nm (pim-O-glucosylcimifugin, liquiritin, 5-O-methylvisammioside) and 250 nm (amonium glycyrrhizinate). The column temperature was 30℃, and sample size was 10 μ L. RESULTS: The linear ranges of prim-O-glucosylcimifugin, liquiritin, 5-O-methylvisammioside and amonium glycyrrhizinate were 6. 138-122. 77 μg/mL (r=0. 999 9), 2. 502-50. 03 μg/mL (r=0. 999 9), 5. 988-119. 75 μg/mL (r=0. 999 9) and 12. 788-255. 76 μg/mL (r=0. 999 9), respectively. RSDs of precision, stability and reproducibility tests were all lower than 2. 0％ (n=6). The recovery rate were 100. 32％ (RSD=0. 58％, n=6), 100. 24％ (RSD=0. 56％, n=6), 101. 28％ (RSD=0. 91％, n=6) and 101. 48％ (RSD=0. 79％, n=6), respectively. Total contents of 4 components in enterprise A were generally higher than enterprises B, C, among which the difference of liquiritin was significant; the content of prim-O-glucosylcimifugin in enterprise B was higher than enterprises A, C, while the content of 5-O-methylvisammioside was lower than enterprises A, C. The content of liquiritin in enterprise B was outlier. CONCLUSIONS: This method is simple, reproducible and can provide reference for quality control of Xinyi biyan pills.
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In this experiment, rat nasal mucosa absorption characteristics of prim-O-glucosylcimifugin and 5-O-methylvisammioside were studied to provide a basis for drug delivery of Toutongning nasal spray. The nasal mucosa absorption test in rats was conducted with in situ nasal perfusion method after pH 6 buffer solution was used to prepare high, medium and low concentrations of prim-O-glucosylcimifugin, 5-O-methylvisammioside mixed solution as liquid circulation in nasal cavity. Then the concentrations of the circulating liquid compositions to be measured were determined by HPLC, and the absorption rates of prim-O-glucosylcimifugin and 5-O-methylvisammioside under different pH conditions were also investigated. According to the results, the absorption rate constant was (0.588±0.041)×10⁻³, (0.547±0.023)×10⁻³, (0.592±0.063)×10⁻³ min⁻¹ for prim-O-glucosylcimifugin high, middle and low concentrations, and (0.438±0.041)×10⁻³, (0.407±0.023)×10⁻³, and (0.412±0.063)×10⁻³ min⁻¹ for 5-O-methylvisammioside high, middle and low concentrations. There was no significant difference among high, middle and low concentration groups, and the absorption under pH 6 was better than that under other pH conditions. Therefore, we can get the conclusion that the main active ingredient of Toutongning nasal sprays can be absorbed through the nasal mucosa, and it is feasible to make nasal spray; in addition, pH 6 of nasal spray is scientific and reasonable.
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Objective: To establish an HPLC method for the determination of gastrodin, prim-O-glucosylcimifugin, 5-O-methylvisammioside, imperatorin and isoimperatorin in Yuzhen powder.Methods: A Phenomenex Gemini C18 column(250 mm×4.6 mm, 5μm) was used and the column temperature was 25℃.The flow rate was 1.0 ml·min-1 and the mobile phase consisted of methanol-water with gradient elution.The detection wavelength was 230 nm and the sample size was 5 μl.Results: The linear range of gastrodin was 2.68-214.0 μg·ml-1(r=0.999 9), and the average recovery was 100.2%(RSD=0.9%, n=6);the linear range of prim-O-glucosylcimifugin was 5.22-418.0 μg·ml-1(r=0.999 7), and the average recovery was 99.9%(RSD=0.9%, n=6);the linear range of 5-O-methylvisammioside was 4.57-365.8 μg·ml-1(r=0.999 5), and the average recovery was 99.7%(RSD=1.0%, n=6);the linear range of imperatorin was 5.22-417.2 μg·ml-1(r=0.999 6), and the average recovery was 99.0%(RSD=0.9%, n=6);the linear range of isoimperatorin was 5.29-423.2 μg·ml-1(r=0.999 8), and the average recovery was 100.2%(RSD=0.8%, n=6).Conclusion: The method is simple and accurate, and the contents of the five ingredients can be determined simultaneously.The method can be used for the quality control of Yuzhen powder.
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Objective: To establish an HPLC method for the simultaneous determination of catalpol, liquiritin, ammonium glycyrrhizinate, asarinin, verbascoside, atractylodin, ferulic acid, imperatorin, notopterol, isoimperatorin, baicalin, prim-O-glucosylcimifugin, and 5-O-methylvisammioside in Jiuwei Qianghuo Oral Liquid (JQOL). Methods: The analysis was performed on Zorbax Eclipse XDB-C18 column (250 mm×4.6 mm, 5 μm) by gradient elution of acetonitrile-0.005 mol/L KH2PO4 (adjusting to pH 3.0 with phosphoric acid) (15:85). The flow rate was 1.0 mL/min. Results: The linear ranges of catalpol, liquiritin, ammonium glycyrrhizinate, asarinin, verbascoside, atractylodin, ferulic acid, imperatorin, notopterol, isoimperatorin, baicalin, prim-O-glucosylcimifugin, and 5-O-methylvisammioside were 2.08-31.22 μg/mL (r=0.9995), 4.01-60.15 μg/mL (r=0.9992), 10.09-151.31 μg/mL (r=0.9992), 4.98-74.63 μg/mL (r=0.9994), 2.05-30.74 μg/mL (r=0.9996), 4.10-61.46 μg/mL (r=0.9996), 2.93-43.98 μg/mL (r=0.9993), 2.04-30.66 μg/mL (r=0.9995), 12.54-181.55 μg/mL (r=0.9997), 53.95-89.23 μg/mL (r=0.9995), 12.05-180.68 μg/mL (r=0.9995), 5.97-89.51 μg/mL (r=0.9994), and 7.99-119.82 μg/mL (r=0.9996). The average recoveries (n=6) were 98.8% (RSD=1.9%), 98.6% (RSD=1.8%), 101.2% (RSD=1.5%), 99.4% (RSD=0.8%), 100.1% (RSD=0.6%), 99.7% (RSD=0.9%), 98.9% (RSD=1.2%), 99.4% (RSD=2.0%), 100.5% (RSD=1.6%), 98.7% (RSD=0.8%), 101.2% (RSD=1.4%), 98.3% (RSD=1.5%), and 99.1% (RSD=1.7%), respectively. The contents of nine batches of the catalpol, liquiritin, ammonium glycyrrhizinate, asarinin, verbascoside, atractylodin, ferulic acid, imperatorin, notopterol, isoimperatorin, baicalin, prim-O-glucosylcimifugin, and 5-O-methylvisammioside were 0.229-0.259 mg/L, 1.231-1.260 mg/L, 0.849-0.877 mg/L, 0.357-0.371 mg/L, 0.149-0.169 mg/L, 0.941-0.967 mg/L, 0.529-0.547 mg/L, 0.269-0.294 mg/L, 1.039-1.067 mg/L, 0.043-0.064 mg/L, 3.631-3.649 mg/L, 0.157-0.183 mg/L, and 0.068-0.084 mg/L. Conclusion: This method is simple and rapid, and can be used for the quality control of JQOL with satisfactory separation and repeatability.
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Objective: To develop an HPLC method for the simultaneous determination of five active components ( 5-O-methyl-visammioside, prim-O-glucosycimifugin, hesperidin, rosmarinic acid and forsythin) in Sijiganmao tablets. Methods:The samples were separated on an Agilent C18 column (250 mm × 4. 6 mm,5 μm) by acetonitrile-0. 1% formic acid solution with gradient elution. The detection wavelength was 283nm,the flow rate was 1. 0μl·min-1 ,the column temperature was 30℃,the detection wavelength was 283 nm,and the sample size was 10μl. Results:The complete separation was obtained for the five active compounds. The five regression e-quations showed good linear relationships. The average recoveries of the compounds were between 95. 0% and 105. 0%. Conclusion:The established method is accurate, reliable, simple and effective, which can be used in the quality control of Sijiganmao tablets.
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Qi She Pill (QSP) is a traditional Chinese medicine (TCM) prescription that has been used in treating cervical spondylosis radiculopathy for many years. In this study, a simple and sensitive method using ultra-high-performance liquid chromatography-tandem mass spectrometry (UHPLC-MS/MS) on a reverse-phase C18 column was developed for the simultaneous determination of the 19 major components in QSP. We found that the optimum mobile phase for gradient elution was 0.1% formic acid and methanol. The correlation coefficients of all calibration curves were greater than 0.99. Recoveries measured at three concentration levels varied from 95.43% to 102.35%. Relative standard deviations of intra- and inter-day precisions were less than 4.45%. After successfully validating our method, we then applied it to the quantification of 19 components in QSP products to show that this method provides a new standard in quality assessment of TCM prescriptions containing multiple bioactive components.
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Objective:To simultaneously determine the contents of asarinin, prim-O-glucosylcimifugin and 5-O-methylvisammio-side in Xinqin granules. Methods:An HPLC method was used. The determination was performed on a ZORBAX Eclipse XDB-C18 col-umn(150 mm ×4.6mm,5 μm) with the mobile phase consisting of menthol (A)-water (B) with gradient elution. The flow rate was 1. 0 ml·min-1 . The column temperature was 30℃. The detection wavelength was set at 254 nm from 0 to 30 min and 287nm from 30 to 55 min. The injection volume was 10μl. Results:The linear range of prim-O-glucosylcimifugin, asarinin and 5-O-methylvisammio-side was 10.210-163.400 μg·ml-1(r=0.999 7),10.160-162.600 μg·ml-1(r=0.999 8) and 5.015-80.240 μg·ml-1(r=0. 999 8), respectively. The average recovery was 100. 30%(RSD=1. 6%, n=6),101. 53%(RSD=1. 1%,n=6) and 101. 12%(RSD=1. 2%, n=6), respectively. Conclusion: The method is simple and accurate, which can be used in the quality control of Xinqin granules.
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Object To establish the quality standard for Wuhu Powder. Methods Radix Angelicae Sinensis (RAS), Radix Angelicae Dahuricae (RAD), and Flos Carthami (FC) were determined qualitatively by TLC. The content of cimicifugoside and 5-O-methylvisammioside were determined by HPLC. Results The linear ranges of cimicifugoside and 5-O-methylvisammioside were 0.370 0—1.850 0 ?g and 0.191 0—0.955 0 ?g. The recoveries were 100.74% and 98.33%, RSD were 0.67% and 1.91% (n=5), respectively. Conclusion The method is simple, accurate, credibility, which can be used as the quality control standard of Wuhu Powder.