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AIM To explore the biotransformation of compound 7-(4-chlorbenzyl)-7,8,13,13a-tetrahydroberberine in the rabbit. METHODS Analyze the rabbit bile sample with HPLC, LC/MS and LC/NMR. RESULTS A metabolite and unchanged 7-(4-chlorbenzyl)-7,8,13,13a-tetrahydroberberine were found in the rabit bile, the metabolite was characterized and its structure was elucidated. CONCLUSION Compound 7-(4-chlorbenzyl)-7,8,13,13a-tetrahydroberberine is metabolized by demethylation at 10-OCH3 position.
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AIM To study the phase I metabolites of phenoprolamine hydrochloride (DDPH) in rat bile. METHODS DDPH was administered ip to bile duct-cannulated rats. Bile samples were collected before administration and up to 12 h after administration. After being treated with β-glucuronidase, the bile samples were purified and enriched with C-18 SPE columns, and then were analyzed by LC/DAD/MSD. The samples containing synthesized reference standards of DDPH metabolite 1-(2,6-dimethylphenoxy)-2-(3-methoxy-4-hydroxyphenylethylamino)-propane (M1), 1-(2,6-dimethyl-3-hydroxyphenoxy)-2-(3,4-methoxy-phenylethylamino)-propane (M2), 1-(2,6-dimethyl-4-hydroxyphenoxy)-2-(3,4-methoxyphenylethylamino)-propane (M3), 1-(2,6-dimethyl-4-hydroxyphenoxy)-2-(3-hydroxy-4-methoxyphenylethylamino)-propane (M4), 1-(2,6-dimethyl-3-hydroxyphenoxy)-2-(3-hydroxy-4-methoxyphenylethylamino)-propane (M5) and 1-(2,6-dimethyl-4-hydroxyphenoxy)-2-(3-methoxy-4-hydroxyphenylethylamino)-propane (M6) were analyzed by LC/DAD/MSD under identical conditions. RESULTS The retention times, UV spectra, molecular weights and production spectra (obtained by collision-induced dissociation)of the apparent ions of peak A, B, C, D, E and F in the total ion chromatogram of DDPH treated rat bile sample were consistent with those of M1, M2, M3, M5, M4 and M6, respectively. CONCLUSION M1, M2, M3, M4, M5 and M6 were identified as the phase I metabolites of DDPH in the rat.
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OBJECTIVE To establish a GC method for the determination of the contents of Pd-Ⅰa and Pd-Ⅱ in roots of Peucedanum Praeruptorum.METHODS The determination was performed on a silica capillary SE-30(0.25 μm 0.22 mm×25 m)column by FID detector;with n-C25H52 as the internal standard.RESULTS The standard curves of Pd-Ⅰa and Pd-Ⅱ were linear over the range from 0.175 μg to 1.919 μg(r=0.9995) and 0.086 μg to 0.950 μg (r=0.9996),respectively.The average recoveries were (98.28±2.07)% for Pd-Ⅰa and (99.58±2.44)% for Pd-Ⅱ.Compared with HPLC,there was no significant difference in the results between GC and HPLC.CONCLUSION The method appeared to be simple,sensitive,rapid and accurate and can be used for the quality control of Chinese medicine Qianhu.
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Objective To establish a stable and reliable HPLC method and fingerprint reference substance for the measurement of the fingerprint, the practical quality control, and assay of the water-soluble components of Salvia miltiorrhiza. Methods The HPLC was run on C 18 columns with methanol-1.0 % glacial acetic acid solution as mobile phase in gradient elution mode at a flow rate of 1.0 mL/min. The chromatographic system suitability, the gradient elution mode, mobile phase acidity, and the effect of column type on fingerprint repeatability were tested. Results The HPLC fingerprints of the water-soluble extract of reference S. miltiorrhiza were obtained with very good resolution under the established chromatographic system. Fifteen peaks in the chromatograms were selected for the fingerprint identification and quality control of S. miltiorrhiza. The quality of ten batches of S. miltiorrhiza samples from different hibitats were assessed by comparing their chromatographic fingerprints with the reference fingerprints obtained at the same time, and the similarity showed no difference, eventhough the column filler was changed. Conclusion Because the inherent complexity of medicinal material components has been reflected by chromatographic fingerprints, there are many factors affecting the fingerprint repeatability for the changes of column type. The results of the quality assessment of S. miltiorrhiza, using fingerprints from different columns, are not all coincidence. In order to obtain the comparable and repeatable results in different laboratories, it is much practical with both a defined chromatographic system suitability and a fingerprint reference substance.
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Object To establish the standardization and digit ization methods for gas chromatographic fingerprint chromatograms of the essenti al oil of Curcuma longa L. Methods A polynomial regression analysis technique was estab lished for the calculation and prediction of the gas chromatographic retention i ndices by using a series of normal aliphatic hydrocarbons as the reference stand ards. And it was used for the characterization of the features of the gas chroma tographic fingerprint spectra of the essential oil of C. longa. Results It was approved that retention indices of the gas chrom atographic fingerprint spectra obtained at a variety of conditions were stable and reliable with excellent reproducibility, and fairly good ruggedness. It was also much better than the relative retention time indices. Conclusion The fingerprint spectra standard established on t he multiple references basis are much more reasonable and useful for the practic al quality assurance and validation of Chinese herbals.
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Object To develop a new method for the determination of curcumol in essential oil from rhizoma Curcumae L.. Methods The contents of curcumol were determined by high performance capillary gas chromatography with sequential increase of temperature on a HEWLETT PACKARD 5890A gas chromatograph. Results The method can be used to determine curcumol with accuracy at a recovery of 101.4% and RSD of 0.40%. Conclusion The present study provided a satisfactory method for the determination of curcumol, and it was found that its contents in four different species (C. wenyujin, C. longa, C. aeruginose, and C. kwangsiensis) were markedly different.
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Objective To isolate and elucidate the structures of alkaloids in Huangyangning. Methods Alkaloids of Huangyangning were separated with preparative HPLC. The molecular structures were elucidated on the basis of chemical evidences and spectral analyses (UV, IR, MS, 1H-NMR, 13C-NMR, COSY, DEPT, HMQC, and HMBC). Results Cyclovirobuxine D is the major component in Huangyangning and cyclobuxine D and cyclovirobuxine C are the two related alkaloids. Conclusion It is demonstrated that all the Huangyangning alkaloids have the same structural frame with only minor differences in substitution through chromatographic and spectral analyses. Therefore, it is not easy to purify cyclovirobuxine D by using usual column, re-crystallization, or chemical approaches for the existence of the related alkaloids.
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Objective To set up the reference standard of cyclovirobuxine D.Methods Thermal analysis,HPLC/MS,HPLC with terminal wavelength,HPLC with fluorescence derivation and with ultraviolet derivation,TLC and nonaqueous titration methods were applied to determine the content of cyclovirobuxine D control.Results Thermal analysis can not be used to analyse the purity of cyclovirobuxine D ,and HPLC/MS,HPLC with terminal wavelength,HPLC with fluorescence derivation and HPLC with ultraviolet derivation can obtain the same purity.Conclusion The methods used for the assay of cyclovirobuxine D control were practical.
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AIM To study the pharmacokinetic characters following oral administration of colon specific tinidazole tablets in healthy dogs METHOD The plasma and intestine content concentration of tinidazole was determined by RP HPLC method following a single oral dose of 500 mg of two formulations given to each dogs in an open randomized two way crossover design RESULT The main pharmacokinetic parameters of test and reference tablets were as follow: T max : (6 3?1 2) h and (2 4?1 1) h; C max : (46 23?8 93) mg?L -1 and (58 08?14 65) mg?L -1 ; AUC 0-t : (423 21?93 08) mg?h?L -1 and (458 22?112 07) mg?h?L -1 The relative bioavailability of tinidazole colon specific enteric tablets was 92 9%?6 6%. 6 5 h after intake of colon specific tablets, there were a great deal of tinidazole in dogs colon but almost no tinidazole in small intestine CONCLUSION The result demonstrated that the colon tropic effect of the tablets is significant in dogs
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The arterial supply of the human odontoid process was studied in 48 cadavers of different ages by dissection, clearing, and radiologic methods. The results were as follows:1. The odontoid process obtains its blood supply directly from the anterior and posterior ascending arteries arising from the vertebral artery and indirectly from the horizontal arteries arising from the ascending pharyngeal artery. Around the odontoid process these arteries form a peculiar anastomosis, the upper part of which is called the apical arch.2. There are two groups of nutrient arteries, the basal and the apical nutrient arteries, in the odontoid process. The basal nutrient arteries penetrate into the process at the base through the anterolateral aspect and the central part of the posterior aspect, mostly 1 branch (81.94?3.21％) from either side. The apical nutrient arteries enter it at the apex, and are usually divided into 2 branches (69.44?7.68％). The outer diameters of the basal nutrient arteries in the new horns, the children, and the adults are 0.09～0.15mm, 0.16～0.19mm, 0.24～0.29 mm, and those of the apical nutrient arteries are 0.03～0.06mm, 0.06～0.10mm, and 0.10～0.14 mm respectively.3. The pattern of arterial distribution within the odontoid process varies with the age. In subjects under twelve years the apex of the process has not yet ossified completely, and no anastomosis can be found between the arteries at the base and those at the apex. In adults ossification has been completed. The intraosseous arteries connect with each other and form an anastomosis network, which is most abundant at the base.
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The arterial supply of human cervical vertebral bodies (C_3-C_7) was studied in 74 fresh cadavers of different ages by dissection and translucent preparation.1. The cervical vertebral bodies mainly obtain their blood supply from the vertebral artery, but the lower two (C_6-C_7) also receive their blood supply from the branches of the inferior thyroid, the deep cervical, the costocervical trunk, the highest intercostal and the subclavian artery. These arteries form a ladder-like anastomosis on the anterolateral surface of the vertebral bodies, and a rectangular or hexagonal anastomosis on the dorsal surface.2. The nutrient arteries enter the vertebral body from the anterolateral and dorsal aspects. They can be divided into the central branches which reach the center of the body and the peripheral ones which lie on the peripheral part of the body. Each of the central branches appears as a straight, unbranching stem. Their centrifugal terminals at the center of the body are arborized and extend to the upper, lower, left and right part of the body to supply the central core of the vertebral body which corresponds to the area of the nucleus pulposus. The peripheral branches, short and early branched, supply the peripheral part of the vertebral body which corresponds to the area of the annulus fibrous.3. The number of the central branches on the anterolateral aspect varies between 0-3 and that on the dorsal aspect is 0-2. The number of the peripheral branches on the anterolateral aspect is 2-13 and that on the dorsal aspect is 0-6. These branches anastomose with each other within the body of the vertebra. The end artery only appears in the developing cartilaginous regions of the body.
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The number, size, direction and position of the nutrient foramina were investigated in a total of 351 dry cervical vertebral arches of human adults. The position of the nutrient foramina is on the external and internal aspect of the arch and is more or less located in a fixed area, but the exact spot varies considerably. One foramen is more frequent on either aspect. The average diameters of the foramina on the external and internal aspect are 0.34 mm and0.26 mm respectively. The foramina on the external aspect are directed towards the pediele and those of the internal aspect backward.A total of 120 vertebral arches (except the atlas) in 20 fresh cadavers of different ages were used to demonstrate the nutrient arteries by dissection and translucent preparation. All nutrient arteries entering the foramina on the external aspectarise from the deep cervical artery and those of the internal aspect from spinal branches of the vertebral artery. After penetrating the arches, they divide into anterior and posterior branches. The former then subdivides into several branches leading to the pedicle, transverse process, upper and lower articular process, whereas the latter branches off into the lamina and spinal process. The course and distribution of the intraosseous arteries have close relation with the ossification of the arch.Small periosteal arteries penetrate the arch from the external aspect only and have not been found on the vertebral canal side except in the new borns.