OBJECTIVETo establish an HPLC method for simultaneous determination of nuzhenide, specnuezhenide, wedelolactone and oleanic acid in Erzhiwan.

METHODThe DIKMA C18 (4.6 mm x 200 mm, 5 microm) column was adopted with acetonitrile and 0.1% phosphoric acid solution as the mobile phase and gradient elution. The flow rate was 1.0 mL x min(-1) and the volume of injection was 20 microL. The column temperature was maintained at 30 degrees C and the detective wavelength was set at 215 nm.

RESULTThere were good linear relationships between the peak area and concentration at the range of 2.008-80.32 (r = 0.999 6), 5.872-234.88 (r = 0.999 7) , 0.9-36 (r = 0.999 9), 13.24-529.6 mg x L(-1) (r = 0.999 6) for nuzhenide, specnuezhenide, wedelolactone and oleanic acid, respectively. The average recovery rates of nuzhenide, specnuezhenide, wedelolactone and oleanic acid were 99.25%, 98.70%, 96.23% and 101.5%, respectively, with RSD of less than 3%.

CONCLUSIONThe established method was so easy, rapid and accurate that it can be used as an effective way for quality control of Erzhiwan.

Chromatography, High Pressure Liquid ; methods ; Coumarins ; analysis ; Drugs, Chinese Herbal ; analysis ; Glucosides ; analysis ; Pyrans ; analysis

An HPLC method for determination of scoparone and ayapin was established for investigating the distributed patterns of scoparone and ayapin in 37 species of Dendrobium. The contents of scoparone and ayapin in varied collected samples were determined by the established HPLC method. The pseudo-bulbs sampled were collected according to different growth age of D. thyrsiflorum. The results showed that the contents of scoparone and ayapin were much differently distributed in species of Dendrobium. Only D. thyrsiflorum and D. densfilorum contained both scoparone and ayapin, the content decreased with the growth age. A fewer amount of ayapin was tested in D. loddigesii from Wenshan. The scoparone and ayapin were not determined in the rest species of Dendrobium. The method was concise, sensitive, accurate and reproducible. It could be applied to assay scoparone and ayapin in populations of herbal Dendrobium.
China ; Chromatography, High Pressure Liquid ; Coumarins ; analysis ; Dendrobium ; chemistry ; Drugs, Chinese Herbal ; analysis ; Sesquiterpenes ; analysis

OBJECTIVETo study the chemical constituents of ethyl acetate-soluble fraction from methanolic extract of the roots and rhizomes of Notopterygium incisum .

METHODThe chemical constituents were isolated and purified by various chromatographic methods, and their structures were identified by NMR and MS data analysis.

RESULTFive compounds were obtained and identified as falcarindiol (1), 8-hydroxy-l-methoxy-( Z) -9-heptadecene-4, 6-diyn-3-one (2) angenomalin (3), scopoletin (4), O-methylnotopterol (5).

CONCLUSIONCompound 5 was a new natural product and compounds 2-4 were isolated from the roots and rhizomes of N. incisum for the first time.

Apiaceae ; chemistry ; Coumarins ; analysis ; isolation & purification ; Plant Extracts ; analysis ; isolation & purification ; Plant Roots ; chemistry ; Rhizome ; chemistry

OBJECTIVETo study the chemical constituents from Lobelia chinensis.

METHODThe constituents were extracted with 95% EtOH, partitioned with different solvents, and isolated and purified by silica gel column chromatography and crystallization, their structures were elucidated by physico-chemical properties and spectroscopic data.

RESULTSeven compounds were isolated from the titled plant. They were identified as 5-hydroxy-4'-methoxyflavone-7-O-rutinoside (1), n-butyl-O-beta-D-fructopyranoside (2), 5,7-dimethoxycoumarin (3), cirsiumaldehyde (4), diosmetin (5), 5-hydroxymethyl-2-furancarboxaldehyde (6), and 6-hydroxy-7-methoxycoumarin (7).

CONCLUSIONCompounds 2-4, 6, and 7 were obtained from the titled plant for the first time.

Coumarins ; analysis ; Furans ; analysis ; Lobelia ; chemistry ; Plant Extracts ; chemistry ; isolation & purification

The present study explored the consistency of the content proportions of active components of Aurantii Fructus and analyzed the influencing factors based on three-dimensional multi-component analysis. A total of 839 Aurantii Fructus samples in 65 research articles were analyzed using the three-dimensional multi-component analysis mode. The content data of flavonoid components(naringin, hesperidin, neohesperidin, narirutin, and nobiletin), coumarin components(meranzin and gluconolactone), and alkaloid(synephrine) in 386 samples which met the criteria of 2020 edition of the Chinese Pharmacopoeia were extracted and adjusted to percentages, and the content ratios between components were calculated. The influencing factors of Aurantii Fructus quality were analyzed. The results showed content ratios of components as follows: neohesperidin∶naringin in the range of 0.4-1.2; narirutin∶naringin in the range of 0.02-0.16; hesperidin∶naringin in the range of 0.01-0.3; nobiletin∶naringin in the range of 0.000 588 3-0.069 68; synephrine∶naringin in the range of 0.02-0.042; gluconolactone∶naringin in the range of 0.001-0.01; meranzin∶naringin in the range of 0.000 4-0.035. The quality of Aurantii Fructus was closely related to the origin, variety, harvesting time, and processing method of medicinal materials. Harvesting time had a greater impact on the quality of Aurantii Fructus, and the origin and variety had a certain impact on the quality of Aurantii Fructus. The findings of this study indicated that the ratios between flavonoid components, flavonoids and coumarin components, and flavonoids and alkaloids fluctuated. The production base should optimize the varieties, harvesting period, and processing methods of Aurantii Fructus to provide a scientific basis for the production of high-quality Aurantii Fructus.
Citrus ; Flavonoids/analysis* ; Drugs, Chinese Herbal ; Fruit/chemistry* ; Coumarins/analysis* ; Chromatography, High Pressure Liquid/methods*

OBJECTIVETo study the chemical constituents in the dried roots of Saposhnikovia divaricata (Turcz.) Schischk.

METHODThe chemical constituents were isolated by various column chromatographic methods and structurally elucidated by IR, UV, MS and NMR evidences.

RESULTTwo compounds were obtained and identified as nodakenetin (1) and 8-[4-(beta-D-glucopyrano-sy-loxy)-3-methyl-2-buten-1-yl]oxy-5-methoxy-6,7-furanocoumarin (2), respectively.

CONCLUSIONCompound 2 is a new compound and named sapodivarin.

Apiaceae ; chemistry ; Coumarins ; analysis ; isolation & purification ; Plant Extracts ; analysis ; isolation & purification ; Plant Roots ; chemistry

UHPLC-LTQ-Orbitrap-MS was developed for the identification of chemical constituents in Qingfei Paidu Decoction, which will clarify its material basis. ACQUITY UHPLC HSS T3 chromatography column(2.1 mm×100 mm, 1.8 μm) was used with 0.1% formic acid(B)-acetonitrile(A) as the mobile phase in gradient elution. The decoction was detected by high-resolution liquid chromatography-mass spectrometry equipped with an ESI ion source in positive and negative mode. Based on the accurate mass measurements, retention time, mass fragmentation patterns combined with comparison of reference and literature reports, a total of 87 major compounds including 43 flavonoids, 9 alkaloids, 4 triterpenoid saponins, 1 sesquiterpene, 2 coumarins, 10 phenolic acids and 18 other compounds were tentatively screened and characterized. UHPLC-LTQ-Orbitrap-MS was employed to comprehensively elucidate the chemical components in Qingfei Paidu Decoction, which basically covered 20 Chinese medicines except gypsum in Qingfei Paidu Decoction. These collective results provide a scientific basis for further research on the quality control standard of Qingfei Paidu Decoction.
Chromatography, High Pressure Liquid ; Coumarins ; analysis ; Drugs, Chinese Herbal ; Flavonoids ; analysis ; Mass Spectrometry

AIMTo determine the location and relative quantity of coumarins in the stem of Dendrobium thyrsiflorum Rchb. f. , and to provide a scientific basis for evaluating and utilizing the famous medicinal plant.

METHODSThe stems of one, two and three years old, separately, were collected in February. Location and relative quantity of coumarins in the top, middle and basal parts of each stem sample were determined by using laser scanning confocal microscopy (LSCM). ANOVA and Tukey's test were employed in the statistical analysis.

RESULTSThe coumarins located mainly in vascular bundles, especially on the walls of the outer fiber cells. There was significant difference or great significant difference exist in every part of the stem from different ages. The values of significant difference were as follows: basal part P = 0.004 (< 0.01); middle part P = 0.009 (< 0.01); top part P = 0.036( < 0.05).

CONCLUSIONTwo years old stem could be the best choice when collecting Dendrobium thyrsiflorum in Feburary.

Coumarins ; analysis ; Dendrobium ; chemistry ; Microscopy, Confocal ; Plant Stems ; chemistry ; Plants, Medicinal ; chemistry ; Time Factors

To explore the effect of different processing methods and conditions of coumarin and volatile compounds in Angelica Dahuricae Radix and their change regularity, in order to optimize and establish appropriate drying methods and conditions. After being cleaned, fresh Angelica Dahuricae Radix herbs were baked, sun-dried, shade-dried, sun-dried after sulfur-fumigation, dried by quick-lime embedding, freeze-dried, microwave-dried. Finally, 24 groups of samples were obtained after being mashed and passing through the 60-mesh screen. The HPLC-PDA method was adopted to simultaneously determine the content of coumarin compounds. The GC-MS method was used to determine the content of volatile compounds. The principal component analysis (PCA) was made on the standardized analysis results for the 24 groups of samples processed with different drying methods. According to the PCA results, the comprehensive scores of coumarin and volatile compounds in Angelica Dahuricae Radix herbs processed with different methods in the order from high to low were that unpeeled and dried by quicklime embedding > unpeeled and dried with hot-air at 100 degrees C > unpeeled and dried with hot-air at 40 degrees C > peeled and infrared-dried > peeled and dried with hot-air at 60 degrees C > peeled and dried with hot-air at 40 degrees C > peeled and sun-dried > peeled and dried with hot-air at 60 degrees C > peeled and dried with hot-air at 100 degrees C > peeled and microwave-dried > peeled and dried with hot-air at 80 degrees C > unpeeled and sun-dried > unpeeled and dried with sulfur-fumigation > peeled and dried with sulfur-fumigation > unpeeled and dried with hot-air at 120 degrees C > unpeeled and freeze-dried > unpeeled and infrared-dried > peeled and dried with hot-air at 120 degrees C > peeled and freeze-dried > peeled and dried by quicklime embedding > unpeeled and dried with hot-air at 80 degrees C > peeled and shade-dried > unpeeled and shade-dried > unpeeled and microwave-dried. According to the findings, different drying processing methods have certain impacts on the content coumarin and volatile compounds in Angelica Dahuricae Radix herbs. The traditional method of drying by quicklime embedding is recommended as the optimum origin processing method of Angelica Dahuricae Radix, which is followed by the method for being peeled and dried with hot-air at 100 degrees C.
Angelica ; chemistry ; Coumarins ; analysis ; Desiccation ; methods ; Gas Chromatography-Mass Spectrometry ; Hot Temperature ; Principal Component Analysis ; Volatile Organic Compounds ; analysis

This study is aimed to establish a high-performance liquid chromatography (HPLC) method for simultaneous determination of skimmin, scopolin and umbelliferone in Saussurea hieracioides. Samples were analyzed on a Wondasil C18-WR column (4.6 mm x 250 mm, 5 microm) with methanol (A) and water containing 0.1% phosphate (B) as mobile phases for gradient elution at a flow rate of 1.0 mL x min(-1). The detection wavelength and column temperature were set at 325 nm and 35 degrees C, respectively, and the sample size was 10 microL. The results showed that skimmin, scopolin and umbelliferone were simultaneously achieved within 40 min under the above conditions. A good linearity was observed in the range of 0.18-5.6 microg (r = 1.000 0), 0.060-1.8 microg (r = 0.999 9), 0.032-0.97 microg (r = 0.999 8) for skimmin, scopolin and umbelliferone, respectively, with the average recoveries of 99.16% (RSD = 0.41%), 100.3% (RSD = 0.79%), 102.2% (RSD = 0.87%). The method is simple, accurate and reproducible and can be used for the quality control of S. hieracioides.
Chromatography, High Pressure Liquid ; Coumarins ; analysis ; Glucosides ; analysis ; Medicine, Tibetan Traditional ; Reproducibility of Results ; Saussurea ; chemistry ; Umbelliferones ; analysis