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Objective: To established a rapid nondestructive determination method for the multi-marker constituents in Angelica sinensis by near infrared spectroscopy (NIRS) combined with the partial least squares (PLS) method in order to improve the quality control for A. sinensis. Methods: A total of 108 batches of A. sinensis from different origins were collected for the research. An Ultra performance liquid chromatography (UPLC) method was established to measure the content of the seven components in A. sinensis, which were adopted as the reference value. And the integrating sphere diffuse reflection mode was employed to collect the NIR spectrum. The quantitative calibration model between the near infrared spectrum and the reference content of each component to be measured was established by PLS and other chemometrics methods. Each part of the modeling process was optimized respectively, including the selection of calibration set and validation set, different pretreatment methods and different spectral section. Results: The correlation coefficient for calibration set of chlorogenic acid, ferulic acid, isochlorogenic acid A, ligustilide, butylidenephthalide, senkyunolide I and levistilide A were 0.937 6, 0.970 2, 0.963 4, 0.991 1, 0.962 4, 0.966 6 and 0.947 6, respectively; The root mean square error of prediction (RMSEP) were 0.072 1, 0.038 9, 0.011 3, 0.483 0, 0.017 5, 0.178 0 and 0.097 0, respectively. The predicted values of NIRS models and the measured values of UPLC showed a good linear relation, which presented a great prediction ability of the models. Conclusion: The methods of NIRS combined with PLS can be applied for the rapid content determination of seven components in A. sinensis including chlorogenic acid, ferulic acid, isochlorogenic acid A, ligustilide, butylidenephthalide, senkyunolide I and levistilide A, which is proved to be simple and reliable.
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Objective: To evaluate the feasibility of the application of composite phospholipid liposome-based artificial skin membrane (CPLASM) for measuring biopharmaceutical properties of active fraction extracted from Xiangfu Siwu Decoction (XSD) via transdermal administration. Methods: The HPLC method was established for the determination of active ingredients (ferulic acid, tetrahydrocolumbamine, tetrahydropalmatine, senkyunolide I, and senkyunolide H) in active fraction of XSD. The oil/water partition coefficient values of these active ingredients were measured. The CPLASM was prepared to determine the in vitro permeability parameters of active fraction of XSD. The obtained parameters were further compared with those obtained by porcine ear skin. Results: The oil-water partition coefficients of ferulic acid, tetrahydrocolumbamine, tetrahydropalmatine, senkyunolide I, and senkyunolide H in active fraction of XSD (pH 5.5) were measured to be 1.220 ± 0.280, 0.670 ± 0.085, 0.920 ± 0.110, 1.040 ± 0.092, 1.030 ± 0.093 (n = 3), respectively. The permeability parameters of the active ingredients through porcine ear skin and CPLASM indicated a significant correlation (r > 0.9). Compared with the classical oil-water partition coefficients, the 6 h- cumulative permeation ratio of five active ingredients through CPLASM can be characterized as effectively predicting permeability parameters through porcine ear skin. Conclusion: The biopharmaceutical properties of active fractions from Chinese material medica can be effectively characterized by the application of CPLASM for the determination of in vitro permeability parameters of active ingredients.
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Objective: To optimize the processing technology for prepared Chuanxiong Rhizoma by D-optimal response surface methodology with comprehensive weighted of multi-index. Methods: The single factor experiment was used to optimize the dilution ratio and the moistened time of rice wine. Then, based on the contents of five main components (ferulic acid, ligustilide, senkyunolide A, senkyunolide I, and 3-butylidenephthalide), the D-optimal response surface methodology was used to optimize the rice wine dosage, stir-fried temperature, and stir-fried time in the processing technology for prepared Chuanxiong Rhizoma. Results: The optimal processing technology for prepared Chuanxiong Rhizoma was mixed with 20% rice wine, moistened for 75 min, and stir-fried for 12 min at 156 ℃. Also, it was found that the contents of senkyunolide A, senkyunolide I, and 3-butylidenephthalide in prepared Chuanxiong Rhizoma had increased, and it should be associated with processing. Conclusion: The processing technology for prepared Chuanxiong Rhizoma optimized by D-optimal response surface methodology with comprehensive weighted of multi-index can be used to optimize the process parameters, promote the stability and repeatability of the processing technology, which can significantly control the inner quality of prepared Chuanxiong Rhizoma to ensure effectiveness in clinical application.
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OBJECTIVE: To study the influence and mechanism of bioactive ingredients of Ligusticum chuanxiong Hort. on the transport of gastrodin based on cell culture model in vitro. METHODS: Cell toxicity of gastrodin, ligustilide, senkyunolide I and senkyunolide A were detected by MTT assay. The transport mechanism of gastrodin and the influence of ligustilide, senkyunolide I and senkyunolide A on the transport of gastrodin were studied in MDCK-MDR1 monolayer cells. The changed expressions of P-gp caused by ligustilide, senkyunolide I and senkyunolide A were analyzed by Western blotting. RESULTS: Gastrodin showed relatively poor absorption in MDCK-MDR1 cells for its apparent permeability coefficients were less than 1×10-6 cm·s-1. P-gp inhibitor made the Papp(B→A)/Papp(A→B) of gastrodin reduced from 1.29 to 0.79, which indicated that the transport of gastrodin was influenced by P-gp. In the presence of ligustilide(30 μg·mL-1) or senkyunolide I(120 μg·mL-1), the Papp(A→B) of gastrodin in MDCK-MDR1 were significantly increased(P<0.01). In the presence of senkyunolide A(120 μg·mL-1), the Papp(A→B) of gastrodin in MDCK-MDR1 were markedly increased(P<0.05). High, medium and low dose of ligustilide, senkyunolide A and senkyunolide I could significantly inhibit the expression of P-gp protein. CONCLUSION: The results indicate that the transport mechanism of gastrodin might be passive diffusion as the dominating process with the active transportation mediated mechanism involved. Ligustilide, senkyunolide A and senkyunolide I increase the transport of gastrodin attribute to down-regulate P-gp expression.
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Objective: To investigate the chemical constituents from Guanxinning Injection. Methods: The chemical constituents were repeatedly isolated by column chromatographic techniques including silica gel, ODS, Sephadex LH-20, and macroporous resin, and were purified by preparation HPLC chromatography and recrystallization, and their structures were identified by physicochemical properties and spectroscopic data. Results: Nineteen compounds were isolated and identified as protocatechuic aldehyde (1), vanillin (2), ferulic acid (3), 2-furoic acid (4), senkyunolide I (5), caffeic acid (6), salvianolic acid A (7), isosalvianolic acid A (8), salvianolic acid B (9), isosalvianolic acid C (10), rosmarinic acid (11), 1, 3-dicaffeoylquinic acid (12), senkyunolide H (13), 4-hydroxybenzoic acid (14), m-hydroxybenzoic acid (15), o-hydroxybenzoic acid (16), 4-hydroxycinnamic acid (17), methyl rosmarinate (18), and salvianolic acid N methyl ester (19). Conclusion: Nineteen compounds are isolated from the Guanxinning Injection for the first time, and all HPLC analyses and literature data show that compounds 2, 3, 5, 13-16 are originated from Ligusticum chuanxiong, compounds 7-11, and 18-19 from Salvia miltiorrhiza, and compounds 1, 4, 6, 12, and 17 from L. chuanxiong and S. miltiorrhiza.
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OBJECTIVE: To establish an LC-MS method for simultaneous determination of six compounds (uridine, guanosine, ferulic acid, ligustilide, senkyunolide I and II in Shunaoxin dropping pills. METHODS: The analysis was performed on a Waters Acquity BEH C18 column (2.1 mm × 100 mm, 1.7 μm) with the mixture of acetonitrile-water-formic acid as the mobile phase, and the flow rate was 0.4 mL · min-1; the PDA detection wavelength was 190-400 nm; the column temperature was room temperature (30°C). RESULTS: The linear ranges for uridine, guanosine, ferulic acid, ligustilide, senkyunolide I and H were 10.31-206.24, 3.28-65.52, 6.36-127.24, 8.24-164.88, 10.18-200.52, and 3.14-62.72 μg · mL-1, respectively. The average recoveries were between 99%-101% (n=6). CONCLUSION: This method is simple, accurate and reliable to determine the contents of the six compounds in Shunaoxin dropping pills for the quality control.
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OBJECTIVE: To study the in situ intestinal absorption kinetics of senkyunolide I in rats. METHODS: The absorption of senkyunolide I in four segments of rat intestine was investigated using the in situ single-pass perfusion method, and the drug content was measured by HPLC. The absorption kinetics of senkyunolide I at different segments of intestine, drug concentration, and perfusion medium were studied. RESULTS: Drug concentration had no significant influence on the ka and the P values of senkyunolide I (P≤0.05) in the range of 128.5-514 μg · mL-1 Papp values of senkyunolide 1at duodenum were significantly higher than those atthe other three regions of intestine (P<0.001). But no significant differences in the P value (P≤0.05) were found among jejunum, ileum, and colon. CONCLUSION: The absorption of senkyunolide I complied with linear kinetics in the dose range studied, indicating that its absorption may be mediated mainly by passive transport. Senkyunolide 1could be absorbed at all the studied intestinal segments while duodenum seemed to be the best absorption segment for it.
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AIM: To identify an unknown peak in Guanxinning Injection(Radix et Rhizome Salviae Miltiorrhizae,Rhizoma Chuanxiong) chromatographic fingerprint. METHODS: The elution(44-46 min) separated and collected by HPLC was analyzed by GC-MS and HPLC-PDA-MS-MS. RESULTS: The unknown peak was corresponding to senkyunolidel I. CONCLUSION: It is quick method to identify the reported chemical in herbal medicine based on a small quantity of sample by GC-MS and HPLC-PDA-MS-MS.