The present study established a determination method of Psoraleae Fructus by quantitative analysis of multi-components by the single marker(QAMS) and further improved the thin-layer chromatography(TLC) method. The QAMS method was established by UPLC with psoralen as the internal marker, and the content of psoralenoside, isopsoralenoside, psoralen, and isopsoralen was simultaneously determined. As revealed by the comparison with results of the external standard method, the QAMS method was accurate and feasible. According to the current quality standards of Psoraleae Fructus, the TLC method was further optimized and improved, and bakuchiol was added for identification based on the original TLC method with psoralen and isopsoralen as indicators. This study provides a reference for improving the quality control method of Psoraleae Fructus.
Chromatography, High Pressure Liquid/methods* ; Drugs, Chinese Herbal/analysis* ; Ficusin ; Fruit/chemistry* ; Furocoumarins/analysis* ; Psoralea

Coumarins are the main active components in Psoraleae Fructus. To study the multi-component pharmacokinetics of Psoraleae Fructus, this study established a sensitive and rapid ultra-pressure liquid chromatography coupled to tandem mass spectrometry(UPLC-MS/MS) method for simultaneous determination of psoralen, isopsoralen, psoralenoside, and isopsoralenoside in rat plasma. After validation, the method was applied to the investigation of pharmacokinetics of psoralen, isopsoralen, psoralenoside, and isopso-ralenoside in rats after single and multiple administration of Psoraleae Fructus extract. The results revealed that the exposure of psoralen and isopsoralen in rat plasma was high after a single intragastric administration of Psoraleae Fructus extract, with an AUC_(0-∞) of 443 619-582 680 and 167 314-276 903 ng·mL~(-1)·h~(-1), respectively. Compared with these two compounds, the exposure of psoralenoside and isopsoralenoside was lower with marked gender difference. After 7-day administration of Psoraleae Fructus extract to rats, the AUC_(0-∞) of psoralen and isopsoralen was 29 701-81 783 and 39 234-89 914 ng·mL~(-1)·h~(-1), respectively, which was significantly lower than that at the first day(P<0.05), and that of psoralenoside and isopsoralenoside was 7 360-19 342 and 8 823-45 501 ng·mL~(-1)·h~(-1), respectively. There was no significant gender difference in exposure of psoralenoside and isopsoralenoside in male and female rats. However, the exposure of psoralenoside and isopsoralenoside in male rats was reduced(P<0.05), and the t_(1/2) and mean residence time(MRT) were shortened, suggesting that the removal of these two compounds from the body was accelerated.
Administration, Oral ; Animals ; Benzofurans ; Chromatography, High Pressure Liquid ; Chromatography, Liquid ; Drugs, Chinese Herbal ; Ficusin ; Furocoumarins/analysis* ; Glycosides ; Psoralea ; Rats ; Tandem Mass Spectrometry

A UPLC method has been developed for simultaneous determination of nine furanocoumarins of Angelica dahurics,and was used for quality evaluation of A. dahurica from different habitats. ACQUITY UPLC BEH C18 chromatographic column was employed,the separation was performed with the mobile phase consisting of acetonitrile and water,and the detection wavelength was set at254 nm. This method was used to simultaneously determine the content of xanthotoxol,oxypeucedaninhydrate,byak-angelicin,psoralen,xanthotoxin,bergapten,oxypeucedanin,imperatorin and isoimperatorin in A. dahurica from different habitats. Then,the further quality assessment of the drug was carried out by similarity evaluation,cluster analysis( CA),principal component analysis( PCA),and orthogonal partial least squares discriminant analysis( OPLS-DA). The content order of measured furanocoumarins from high to low was: oxypeucedanin>imperatorin>isoimperatorin>oxypeucedaninhydrate>bergapten>byak-angelicin>xanthotoxin>xanthotoxol>psoralen,with the mean content 2. 844,1. 277,0. 649 2,0. 216 2,0. 129 8,0. 062 68,0. 052 68,0. 019 30,0. 018 19 mg·g-1,respectively. There were difference between the batches of the drug,and the quality was influenced by smouldering sulphur based on the results of chemical pattern recognition and content determination. Finally,six active ingredients were recognized as the quality makers using OPLS-DA method. The validated UPLC fingerprint combined with chemical pattern recognition method can be used in the quality control and evaluation of A. dahurica.
Angelica ; chemistry ; Chromatography, High Pressure Liquid ; Drugs, Chinese Herbal ; standards ; Ecosystem ; Furocoumarins ; analysis ; Quality Control

The chemical constituents from lipophilic parts in the roots of Angelica dahurica var. formosana cv. Chuanbaizhi were studied in this paper. The compounds were separated and purified by repeated column chromatographic methods on silica gel and HPLC, and the chemical structures of compounds were determined by spectral data analyses. Twenty-nine compounds were obtained and identified as isoimperatorin (1), β-sitosterol (2), imperatorin (3), bergapten (4), osthenol (5), xanthotoxin (6), isoimpinellin (7), dehydrogeijerin (8), phellopterin (9), isodemethylfuropinarine (10), 7-demethylsuberosin (11), alloimperatorin (12), xanthotoxol (13), isooxypeucedanin (14), alloisoimperatorin (15), demethylfuropinarine (16), 5-hydroxy-8-methoxypsoralen (17), oxypeucedanin methanolate (18), pabulenol (19), byakangelicin (20), marmesin (21), (+) -decursinol (22), heraclenol (23), oxypeucedanin hydrate (24), marmesinin (25), ulopterol (26), erythro-guaiacylglycerol-β-ferulic acid ether (27), threo-guaiacylglycerol-β-ferulic acid ether (28), and uracil (29). Compounds 5, 8, 11, 18, 21-23, and 26-28 were obtained from the roots of title plant for the first time.
Angelica ; chemistry ; Coumarins ; chemistry ; isolation & purification ; Furocoumarins ; chemistry ; isolation & purification ; Methoxsalen ; chemistry ; isolation & purification ; Phytochemicals ; analysis ; chemistry ; Plant Roots ; chemistry

A HPLC method has been developed in the current investigation for simultaneous determination of three chemical markers of by akangelicin, imperatorin and isoimperatorin in Radix Angelicae Dahuricae. Separation was performed at 30 degrees C. on achromatographic column of Platisil ODS C18 (4.6 mm x 250 mm, 5 μm). The mobile phase was acetonitrile-water. The flow rate was 1.0 mL x min(-1) and the detection wavelength was 254 nm. The results showed that the three chemical markers could be well resolved and that in the selected linear range, all calibration curves of the three chemical markers showed good linearity (R2 ≥ 0.999 8). The recoveries of byakangelicin, imperatorin and isoimperatorin were 100.83%, 100.10% and 103.52%, respectively, and RSD were 1.7%, 0.77% and 0.41% (n = 6), respectively. The data suggested that the developed HPLC method had good reproducibility, robustness, and accuracy, which was suitable for the quality control of Radix Angelicae Dahuricae. Applications of this method showed that the three chemical markers had higher contents in the Bozhou Anhui and Changge Henan than others.
Angelica ; chemistry ; Chromatography, High Pressure Liquid ; methods ; Drugs, Chinese Herbal ; analysis ; Furocoumarins ; analysis ; Plant Roots ; chemistry ; Quality Control

A HPLC method was developed for simultaneouly quantitative analyses of aviprin (1), gosferol (2), 3'R-(+)-hamaudol (3), 3'-O-acetylhamaudol (4) and iso-imperatorin (5) in the rhizome of Angelica polymorpha. The analysis was performed at 25 degrees C on an Agilent Eclipse XDB-C18 analytical column (4.6 mm x 250 mm, 5 microm) with the mobile phase of methanol and H2O in gradient elution [55:45 (0 min)-65:35 (25 min)-95:5 (35 min)]. And the flow rate was 1.0 mL min(-1) with the detection wavelengths of 312 nm (1), 306 nm (2), 300 nm (3), 294 nm (4) and 310 nm (5). Consequently, the reqresion equations were Y = 1.81 x 10(3) X + 7.93 x 10(2) (r = 0.9996), Y = 2.49 x 10(3) X - 2.17 x 10(2) (r = 0.9993), Y = 2.02 x 10(3) X - 1.42 x 10(2) (r = 0.9991), Y = 1.57 x 10(3) X - 0.66 x 10(2) (r = 0.999 7), Y = 2.65 x 10(3) X - 1.47 x 10(2) (r = 0.999 6). And the average recoveries were 99.7% (RSD 0.57%), 100.1% (RSD 1.3%), 100.0% (RSD 1.6%), 99.6% (RSD 1.3%), 99.2% (RSD 0.59%), respectively. The precision, repeatability and stability were all consistent with the request of quantitative analysis. The contents of compound 1-5 in A. polymorpha were determined as 0.525%, 0.044%, 0.046%, 0.043%, 0.15%, respectively. Accordingly, this quantitative analysis method is good for the quality control of A. polymorpha.
Angelica ; chemistry ; Chromatography, High Pressure Liquid ; methods ; Chromones ; analysis ; Coumarins ; analysis ; Drugs, Chinese Herbal ; analysis ; Furans ; analysis ; Furocoumarins ; analysis ; Rhizome ; chemistry ; Ultraviolet Rays

OBJECTIVETo demonstrate the vasodilatation activity of the coumarin-containing Angelica dahurica var. formosana and to further analyze active components in the herb extracts.

METHODS(1) The vasodilatation effects induced by different extracts (cyclohexane, ethyl acetate, acetone, methanol, 95 % ethanol and water) of Angelica dahurica var. formosana on mouse thoracic aorta pre-contracted with phenylephrine were investigated. (2) The amount of imperatorin and isoimperatorin in each extract was measured by high-performance liquid chromatography. (3) The vasodilatation effects of imperatorin and isoimperatorin on mouse thoracic aorta were compared using the same in vitro method. (4) The vasodilatation mechanism of imperatorin in the mouse thoracic aorta pre-contracted with phenylephrine was studied using the methods of denuded endothelium, NG-nitro-L-arginine methylester (L-NAME, a nitric oxide synthase inhibitor), and propranolol.

RESULTS(1) The cyclohexane and ethyl acetate extracts of Angelica dahurica var. formosana decreased the maximal response of phenylephrine-induced mouse thoracic aorta contraction dose-dependently, with 50% inhibiting concentration (IC(50)) values of 35.3+/-12.4 mg/L and 40.5+/-12.0 mg/L, respectively. The vasodilatation effect of imperatorin and isoimperatorin was dose-dependent. (2) The cyclohexane extract, showing the strongest vasodilatation effect, possessed the highest contents of imperatorin (4.09%) and isoimperatorin (0.27%, w/w). There was a correlation between the vasodilatation activity and the contents of imperatorin and isoimperatorin in the extracts. (3) The vasodilatation effect of imperatorin was about 4-fold stronger than that of isoimperatorin. (4) The vasodilatation effect of imperatorin was signifificantly attenuated to 24.88%+/-4.06% in the denuded endothelium group compared with the intact endothelium group. And 1 mmol/L L-NAME reduced the imperatorin-induced vasorelaxation by 32.18 %+/-11.29 %.

CONCLUSIONSThe principal effective component of Angelica dahurica var. Formosana was found to be imperatorin. Imperatorin-induced vasodilatation is at least partially regulated by nitric oxide, and has no correlation to beta-receptor.

Angelica ; chemistry ; Animals ; Chromatography, High Pressure Liquid ; Endothelium, Vascular ; physiology ; Furocoumarins ; analysis ; pharmacology ; Male ; Mice ; NG-Nitroarginine Methyl Ester ; pharmacology ; Nitric Oxide ; physiology ; Phenylephrine ; pharmacology ; Plant Extracts ; pharmacology ; Propranolol ; pharmacology ; Vasodilation ; drug effects

OBJECTIVETo optimize the herb processing process for the total contains of psoralen and isopsoralen and the rate of extract in Psoralea corylifolia by micro-wave herb processing.

METHODThe contains of psoralen and isopsoralen was obtained by HPLC. The micro-wave herb processing process was optimized by the way of uniform design and contour map.

RESULTThe optimum process was:20% as salt concentration, 4h as immerse time, micro-wave strength as strong, 270 seconds as micro-wave time. The absolute error of the predicted value from the models were smaller than 6% and 0. 3% respectively.

CONCLUSIONThe regression models are notable and reasonable, which can forecast results precisely.

Chromatography, High Pressure Liquid ; methods ; Fruit ; chemistry ; Furocoumarins ; analysis ; Microwaves ; Plants, Medicinal ; chemistry ; Psoralea ; chemistry ; Regression Analysis ; Reproducibility of Results ; Technology, Pharmaceutical ; instrumentation ; methods

OBJECTIVETo develop an RP-HPLC method for simultaneous determination of 5 constituents in Fructus Cnidii.

METHODAnalysis was performed on an Alltech C18 (4.6 mm x 250 mm, 5 microm) column. The mobile phases were acetonitrile water and acetic acid with gradient elution. The flow rate was 1 mL x min(-1). The monitoring wavelength was 325 nm and 245 nm. The column temperature was 40 degrees C.

RESULTThe linear response ranges were 1-20 microg x mL(-1) (r = 0.999 9) for xanthotoxin, 1-20 microg x mL(-1) (r = 0.999 9) for isopimpinellin, 11-20 microg x mL(-1) (r = 0.999 8) for bergapten, 100-1 200 microg x mL(-1) (r = 0.999 7) for imperatorin, 100-2 000 microg x mL(-1) (r = 0.999 9) for osthole. The average recoveries were all above 95%.

CONCLUSIONThe method is simple, sensitive and accurate with good reproducibility.

Chromatography, High Pressure Liquid ; methods ; Cnidium ; chemistry ; Coumarins ; analysis ; Fruit ; chemistry ; Furocoumarins ; analysis ; Methoxsalen ; analogs & derivatives ; analysis ; Plants, Medicinal ; chemistry ; Reproducibility of Results

OBJECTIVETo establish scientific and efficient quality control standard of Rhizoma et Radix Notopterygii through two quantitative parameters.

METHODThe contents of isoimperatorin and volatile oils in 29 commercial samples from 22 localities of Rhizoma et Radix Notopterygii were determined by HPLC and the method in the pharmacopoeia respectively. The data were statistically analyzed.

RESULTOnly 3 of 29 samples met the required standard in the Chinese Pharmacopoeia (2005 edition), 87% of samples newly produced in 2005 not met the standard. Statistics showed that the contents of volatile oils and isoimperatorin should reach 1.63% and 0.17% respectively when the samples meet requirement of criterion with more than 80% probability. The contents of volatile oil and isoimperatorin were not significantly different (P < 0.05) in the samples of 2005 and 2003, while the contents of isoimperatorin were significantly different between Notopterygium incisum and N. forbesii samples.

CONCLUSIONSince the criterion of volatile oils in the Chinese Pharmacopoeia (2005 version) for Rhizoma et Radix Notopterygii is too high to satisfy for most Rhizoma et Radix Notopterygii samples, it is suggested to reduce it to 1.6% (mL x g(-1)). The content of isoimperatorin is proposed to add to the quality standard of Rhizoma et Radix Notopterygii as above 0.2% (mg x g(-1)).

Apiaceae ; chemistry ; classification ; China ; Chromatography, High Pressure Liquid ; Furocoumarins ; analysis ; Oils, Volatile ; analysis ; chemistry ; isolation & purification ; Plant Roots ; chemistry ; Plants, Medicinal ; chemistry ; Reproducibility of Results ; Rhizome ; chemistry