A new aurone with anti-inflammatory activity from Cleistocalyx operculatus flower buds / 中国中药杂志

A new compound(Z)-6-hydroxy-4-methoxy-5,7-dimethylaurone was isolated from Cleistocalyx operculatus flower buds. Its structure was identified by spectroscopic data including MS, ¹H-NMR, ¹³C-NMR HSQC and HMBC. A known compound, 2',4'-dihydroxy-6'-methoxy-3'5'-dimethylchalcone (DMC), was also isolated and identified,and used as material to synthesize (Z)-6-hydroxy-4-methoxy-5,7-dimethylaurone.Anti-inflammatory activities of the two compounds were tested . The results showed that (Z)-6-hydroxy-4-methoxy-5,7-dimethylaurone possesses much stronger PGE₂ inhibitory activity (IC₅₀ 6.12 nmol·L⁻¹) than the positive control ibuprofen （68.66 nmol·L⁻¹）.

Simultaneous determination of eleven components in Ginkgo biloba leaves by high performance liquid chromatography method / 中国中药杂志

To study Ginkgo biloba leaves in different producing area, we establish an HPLC method for the simultaneously determination of seven flavonoids glycosides and four biflavonoids in G. biloba leaves. The analysis was performed on an Agilent ZORBAX SB-C₁₈ column(4.6 mm×250 mm, 5 μm) wich acetonitrile, and 0.4% phosphoric acid as mobile phase at flow rate of 1 mL•min⁻¹ in a gradient edution, and the detection was carried out at 254 nm.The calibration curves of the seven flavonoids glycosides and four biflavonoids had a good linearitiy with good recoveries. The established HPLC method is simple, rapid, accurate, reliable, and sensitive, and can be applied to the identification and quality control of G. biloba leaves.

Simultaneous determination of thirteen components in Tong'an injection by LC-MS/MS / 中国中药杂志

The aim of this study was to develop a simple, sensitive ultra performance liquid chromatography mass spectrometry (UPLC-MS/MS) method for the determination of syringaresinol, N-trans-feruloyltyramine, chelerythrine chloride, sinomenine, coptisine chloride, sanguinarine, chelidonine, magnolflorine, allocryptopine, protopine, farrerol, stylopine and dihydrosanguin-arine in Tong'an injection (TAI), which could be used for the quality control of TAI. The UPLC analysis was performed on Agilent Zorbax SB-Aq column (2.1 mm×150 mm,3.5 μm), with 0.1% formic acid solution (A) -acetonitrile (B) as the mobile phase for gradient elution (0.01-2 min, 5%B; 2-8 min, 5%-30%B; 8-11 min, 30%-95%B; 11-13 min, 95%B; 13-13.1 min, 95%-5%B; 13.1-14 min, 5%B). The flow rate was 0.5 mL•min⁻¹, and the column temperature was 25 ℃; multiple reaction monitoring (MRM) was performed in electrospray ion source positive ion mode for quantitative determination. The calibration curves for the above thirteen compounds showed good linear relationship in corresponding mass concentration range (r>0.999 0). The average recovery rate of the compounds ranged from 95.70% to 104.8%, with RSD of less than 1.9%. The contents of thirteen active components in 10 batches of TAI were 0.021 2-0.029 0, 0.001 7-0.002 3, 0.000 9-0.001 3, 5.952-6.205 2, 0.195 4-0.240 5, 0.002 0-0.002 9, 0.693-0.798 2, 0.069 3-0.078 2, 0.089 29-0.102 9, 0.386 5-0.420 1, 0.014 3-0.015 9, 0.755 3-0.842 1, and 0.008 2-0.011 2 g•L⁻¹ respectively. Methodology validation proved that this method was simple, rapid, sensitive and accurate, which can be used to provide reference for the comprehensive evaluation of TAI quality. The determination results of 10 batches of TAI showed the content of each batch had no significant difference. The results may provide a basis for the quality control of TAI.

Effect of rat intestinal flora in vitro on metabolites of acteoside / 中国中药杂志

Acteoside was used for anaerobic incubation with rat intestinal flora in vitro. HPLC was used to detect the changes of acteoside at different incubation time points and HPLC-Q-TOF-MS was used to identify the metabolites of acteoside. The results showed that acteoside could be metabolized by rat intestinal flora in vitro and the metabolites were 3,4-dihydroxyphenyl acid, caffeic acid and 3-(3'-hydroxyphenyl) propionic acid.

Effect of rat intestinal flora on in vitro metabolic transformation of pumiloside / 中国中药杂志

To study the metabolic transformation of pumiloside by rat intestinal flora in vitro and identify its metabolites. Pumiloside was incubated in the rat intestinal flora in vitro. HPLC was used to monitor the metabolic process, and HPLC-Q-TOF-MS was used to identify the structures of biotransformation products. In vitro, pumiloside was easily metabolized by rat intestinal flora, and with the prolongation of metabolic time, pumiloside was transformed into several metabolites. Three metabolites were initially identified in this experiment. The study indicated that pumiloside could be extensively metabolized in the rat intestinal flora in vitro.

Research on Chinese medicine pairs effects of Panax notoginseng and Bletilla striata before and after compatibility on contents of notoginsenosides / 中国中药杂志

To discuss the synergistic mechanism of compatible use of two medicinal herbs,Panax notoginseng and Bletilla striata, an HPLC was established to determine two ginseng saponins (20S)-ginseng saponin Rg₃ and ginseng saponin Rh₄ contained in single decoction of Panax notoginseng as well as in compound decoction of Panax notoginseng and Bletillastriata in different compatibility ratio (1∶0.5, 1∶1, 1∶2), followed by analyzing the impact of amount of notoginsenosides after compatibility. As a result, compared with the single decoction of Panax notoginseng, the contents of ginseng saponin Rg₃ and ginseng saponin Rh₄ in the compound decoction of Panax notoginseng and Bletillastriata were on the rise as the increasement of the amount of Bletillastriata. The contents of the notoginsengsaponin R₁, ginseng saponin Rg₁ and ginseng saponin Rb₁ of Panax notoginseng single decoction were significantly decreased after compatibility. Therefore, after compatibility, it was more easy to produce (20S)-ginseng saponin Rg₃ and ginseng saponin Rh₄.This study can extend to a method of preparation of (20S)-ginseng saponin Rg₃ and ginseng saponin Rh₄. Furthermore, after compatibility, two ginseng saponins which had lipase inhibitory effect were both increased significantly, indicating that the compatibility of these two herb medicines may have effect on losing weight.

Study on chemical constituents from seed of Oroxylum indicum / 中国中药杂志

Oroxylum indicum was a traditional Chinese medicine. In order to study the chemical constituents from the seed of O. indicum, the chemical constituents of 80% methanol extract of seeds of O. indicum were subjected to chromatography on silica gel, Sephadex LH-20, and preparative HPLC, leading to the isolation of eleven compounds. The structures were identified by various spectroscopic data including ESI-MS, 1H-NMR and 13C-NMR data as oroxin B (1), chrysin (2), baicalein (3), neglectein (4), quercetin-3-O-β-D-galactopy ranoside (5), quercetin-7-O-β-D-glucopyranoside (6), 2α,3β-dihydroxylluPeol (7), lupeol (8), rengyol (9), β-sitostero (10), and stigmasterol (11). Among them, compound 5 were firstly obtained from O. indicum.

Traditional Chinese medicine pairs (III)--effect of extract of Ginseng Radix et Rhizoma and Puerariae Lobatae Radix on intestinal absorption in rats / 中国中药杂志

This study focused on the intestinal absorption of traditional Chinese medicines (TCM) to reveal the scientific connotation of the compatibility of TCM pairs. The single pass intestinal perfusion (SPIP) was used in rats to compare the absorption of single extracts from Puerariae Lobatae Radix, single extracts from Ginseng Radix et Rhizoma, combined extracts from Puerariae Lobatae Radix and Ginseng Radix et Rhizoma and Puerariae Lobatae Radix and Ginseng Radix et Rhizoma mixture in rats. The content of puerarin, ginsenoside Rg1, ginsenoside Re and ginsenoside Rb1 in liquid were tested by HPLC. The speed constant (Ka) and apparent permeability coefficients (Papp) were calculated and compared. Specifically, the order of puerarin Ka and Papp values from high to low was Ginseng Radix et Rhizoma and Puerariae Lobatae Radix mixture > single extracts from Puerariae Lobatae Radix > combined extracts from Ginseng Radix et Rhizoma and Puerariae Lobatae Radix; the order of ginsenosides Ka and Papp values from high to low was Ginseng Radix et Rhizoma and Puerariae Lobatae Radix mixture > single extracts from Ginseng Radix et Rhizoma > combined extracts from Ginseng Radix et Rhizoma and Puerariae Lobatae Radix. The combined administration of Ginseng Radix et Rhizoma and Puerariae Lobatae Radix may improve the absorption in the intestinal tract.

Rapid determination of four components in Guizhi Fuling capsule with online two-dimensional liquid chromatography / 中国中药杂志

To establish the online two-dimensional liquid chromatography by using double gradient liquid chromatography system and UV detector, in order to simultaneously determine the content of paeoniflorin, paenol, amygdaloside and cinnamic acid. A pump of the two-dimensional liquid chromatography was adopted as the one-dimensional separation pump. C18 (3.0 mm x 150 mm, 3 microm) was used as the analytical column, with acetonitrile as the organic phase and 0.08% phosphoric acid + 0.08% triethylamine as the aqueous phase for gradient elution at the flow rate of 0.5 mL x min(-1). Another pump of the two-dimensional liquid chromatography was adopted as the two-dimensional separation pump. PAII C18 was used as the analytical column, with acetonitrile as the organic phase and 20 mmol, pH 3.0 monopotassium phosphate as the aqueous phase for gradient elution at the flow rate of 0.8 mL x min(-1). The detection wavelengths were set at 218, 230, 275 nm by using wavelength time-switching program. The linearity range of paeoniflorin, amygdaloside, paeonol and cinnamic acid were 5.55-222 (r = 0.999 7), 6.6-264 (r = 0.999 8), 3.3-132 (r = 0.999 5) and 0.315-12.6 mg x L(-1) (r = 0.999 7), respectively. The average recoveries of the four components were between 96.12% and 103.9%. The experiment proved that this method was so rapid and accurate in determination results that it could be used for evaluating drug quality.

Transformation of strictosamide to vincoside lactam by acid catalysis / 中国天然药物

AIM@#To identify the structure of the acid-catalyzed product of strictosamide and explore the reaction mechanism.@*METHODS@#The acid-catalyzed reaction process of strictosamide was monitored by HPLC, and a macroporous resin was used to purify the reaction solution. The structure of the product was confirmed by MS, NMR, and ROESY spectra.@*RESULTS@#The acid-catalyzed transformation yield from strictosamide to vincoside lactam was 52%.@*CONCLUSION@#The reaction mechanism of the transformation from strictosamide to vincoside lactam may be related to the stability of the three-dimensional configuration of the compound. These results offer a new way to obtain vincoside lactam from the widely distributed indole alkaloid strictosamide by acid-catalysis.

Quality evaluation of domestic Echinacea extracts / 中国中药杂志

<p><b>OBJECTIVE</b>To determine the content of polyphenol contained samples, in order to provide basis for comprehensive quality evaluation on Echinacea extracts.</p><p><b>METHOD</b>LC-MS was used for qualitative analysis on relevant compounds of the samples of Echinacea extracts. Optimized USP methods, RP-HPLC and QAMS (quantitative analysis of multi-components by single-marker) were used to determine the content of polyphenol. Meanwhile, UV method was adopted for comparative analysis on content according to international standard IS014502-1-2005.</p><p><b>RESULT</b>The six batches of samples could not meet the export standard for polyphenol content by HPLC. UV showed four batches in line with the standard and two batches in inconformity.</p><p><b>CONCLUSION</b>UV method is generally adoptedfor the content determination of domestic Echinacea extracts, but shows results that are significantly different from that by HPLC method. it is suggested to use HPLC method to standardize quality of extracts and raise market access standards.</p>

Orthogonal test for preparing genipin with enzymolyzed geniposide / 中国中药杂志

<p><b>OBJECTIVE</b>To optimize the process for preparing genipin with enzymolyzed geniposide by an orthogonal experiment.</p><p><b>METHOD</b>The optimal enzymolysis process was selected by an orthogonal experiment, with the concentration of geniposide as the index as well as enzyme quantity, pH of enzymolysis solution, enzymolysis time and enzymolysis temperature as considerations.</p><p><b>RESULT</b>The optimal hydrolysis conditions were as follow: rough genipin samples at the concentration of 40 g x L(-1) were selected and shook on a table concentrator at a speed of 100 r x min(-1), added with beta-glucosidase-geniposide 1 : 1 (weight proportion), with pH of enzymolysis solution at 4.5, hydrolyzation temperature at 50 degrees C, the conversion rate of genipin could reach 85.8%.</p><p><b>CONCLUSION</b>The process is so stable and feasible that it can provide theoretical basis for the preparation of genipin with enzymolyzed geniposide.</p>