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A novel, simple and efficient capillary electrophoresis method was developed to simultaneous determination of six furanocoumarins (psoralen, isopsoralen, imperatorin, isoimperatorin, phellopterin, and cnidilin). The separation buffer consisted of 30 mM boric acid, 12 mM sulfobutylether-β-cyclodextrin and 1.5 mM 2-hydroxypropyl-β-cyclodextrin (pH 7.8); the voltage was 20 kV, the temperature was 25 °C and the detection wavelength was at 246 nm with a diode array detector (DAD). Under the above conditions, the analytes could be separated with high resolution in less than 7 min. This method was used to simultaneously determine the content of psoralen, imperatorin, isoimperatorin and phellopterin in Angelica Dahurica Radix. And good linearities were obtained with correlation coefficients from 0.9992 to 0.9999. The limits of detection (LOD, S/N = 3) and the limits of quantitation (LOQ, S/N = 10) ranged from 0.6 to 3.0 μg/mL and from 2.1 to 9.9 μg/mL, respectively. The recoveries ranged between 98.8% and 101.8%. The results indicated the method can achieve baseline separation and quantitative analysis of furanocoumarins in Chinese herbal medicines and formulations., Competing Interests: Declaration of competing interest The authors have declared no conflict of interest., (Copyright © 2022 Elsevier Inc. All rights reserved.)

Bufei-Huoxue Capsule (BFHX) was applied to treat chronic obstructive pulmonary disease (COPD) in China. It is composed of Astragali Radix, Paeoniae Radix Rubra, and Psoralea Fructus. A sensitive and reliable ultra-high-performance liquid chromatography-mass spectrometry (UHPLC-MS/MS) method was developed and validated to quantify the eight main bioactive compounds (psoralen, isopsoralen, neobabaisoflavone, corylin, bavachin, astragaloside IV, ononin and formononetin) in rat plasma after oral administration of BFHX. Osthol was used as an internal standard (IS). Plasma samples were pretreated with methanol to precipitate protein. Chromatographic separation was accomplished using Hypersil GOLD TM C18 column (2.1 mm × 100 mm, 1.9 μm) with a gradient elution profile and a mobile phase consisting of (A) 0.1% formic acid in water and (B) acetonitrile and the flow rate was set at 0.2 mL/min. Multiple reaction monitoring (MRM) mode was applied to perform mass spectrometric analyses. All calibration curves were linear (r > 0.9908) in tested ranges. The intra- and inter-day accuracy and precisions of eight compounds at three different concentration levels were within the acceptable limits. The extraction recovery was within the range of 76.4 ∼ 105.2% and the matrix effects were within the range of 88.3 ∼ 115.0% (RSD ≤ 15.6%). The dilution effects were within the range of 90.2 ∼ 114.9%. These 8 compounds were stable under the tested conditions. So the developed method was valid to evaluate the pharmacokinetic study of eight bioactive compounds after oral administration of BFHX., (Copyright © 2021 Elsevier B.V. All rights reserved.)

Three new benzolactones (1-3), together with four known ones (4-7), were isolated from the whole herb of Lavandula angustifolia. Their structures were established on the basis of detailed spectroscopic analysis (1D- and 2D-NMR, HRESIMS, UV, and IR) and comparison with data reported in the literature. New compounds were evaluated for their anti-tobacco mosaic virus (TMV) activities and cytotoxic activities. The results revealed that compounds 1-3 showed obvious anti-TMV activities with inhibition rates of 26.9, 30.2, and 28.4%, which were at the same grade as positive control. Compounds 1-3 also showed weak inhibitory activities against some tested human tumor cell lines with IC 50 values in the range of 32.1-7.6 μM.

A series of new furanocoumarins with long-chain hydrophobic groups, namely andafocoumarins A-H and J, have been isolated from the dried roots of Angelica dahurica cv. Hangbaizhi (Angelicae Dahuricae radix) in our previous study, among which andafocoumarins A and B were demonstrated to have better anti-inflammatory activity than the positive controls. In this work, a sensitive, accurate, and efficient ultra-fast liquid chromatography coupled with triple quadrupole mass spectrometer (UFLC-MS/MS) method was developed and validated for simultaneous quantification of above-mentioned nine compounds in four cultivars of Angelicae Dahuricae Radix. Chromatographic separation was performed on a Kinetex 2.6u C18 100 Å column (100 × 2.1 mm, 2.6 µm). The mobile phases were comprised of acetonitrile and water with a flow rate of 0.5 mL/min. Using the established method, all components could be easily separated within 12 min. With the multiple reaction monitor mode, all components were detected in positive electrospray ionization. The method was validated with injection precision, linearity, lower limit of detection, lower limit of quantification, precision, recovery, and stability, respectively. The final results demonstrated that the method was accurate and efficient, which could be used to simultaneously quantify the nine andafocoumarins in Angelicae Dahuricae Radix. The results also indicated that in different batches of Angelicae Dahuricae Radix, some of the andafocoumarins were significantly different in terms of content.

A sensitive, specific and rapid ultra-high-pressure liquid chromatography tandem mass spectrometry (UHPLC-MS/MS) method has been developed to investigate pharmacokinetic properties of psoralen and isopsoralen, two compounds isolated from raw/salt-processed fruit of Psoralea corylifolia L. UHPLC-MS/MS was used with positive ion electrospray. The mobile phase was composed of acetonitrile and 0.1% formic acid aqueous solution and a gradient elution program at flow rate of 0.3 mL/min was applied. Multiple reaction monitoring mode was used for the quantification of psoralen, isopsoralen ([M + H](+) m/z 187.0 → m/z 131.0) and scoparone (m/z 207.0 → m/z 151.1). Scoparone served as an internal standard. The method was fully validated for its sensitivity, selectivity, stability, matrix effect and extraction recovery. The obtained results showed that salt-processed Buguzhi significantly promoted the absorption of psoralen and isopsoralen, and increased the bioavailability of these compounds., (Copyright © 2015 John Wiley & Sons, Ltd.)

To study the heating treatment of Angelica dahurica under different temperature and time conditions on the stability of coumarins and tyrosinase activity. HPLC method was used to determine the contents of imperatorin and isoimperatorin, and tyrosinase activity was assayed by measuring the oxidation rate of L-DOPA in vitro. After heated, the contents of imperatorin increased. Expect for being heated at 90 ℃ for 2 h, the content of isoimperatorin was higher than crude one. Before and after being heated, A. dahurica showed an activating effect on tyrosinase. In the same temperature and time conditions, the activation rate increased with the rise of concentration of tyrosinase extracts. Heating process for A. dahurica could change the contents of imperatorin and isoimperatorin, mainly increasing their concentrations., Competing Interests: The authors of this article and the planning committee members and staff have no relevant financial relationships with commercial interests to disclose., (Copyright© by the Chinese Pharmaceutical Association.)

Radix Angelicae dahuricae is a well-known medicinal herb in a number of herb preparations for medical uses. In this study, a rapid and selective method using liquid chromatography with tandem mass spectrometry was developed for the separation and simultaneous quantitation of nine furanocoumarins from Radix A. dahuricae, namely imperatorin, isoimperatorin, oxypeucedanin hydrate, bergapten, oxypeucedanin, xanthotoxol, xanthotoxin, isopimpinellin, and psoralen. Chromatographic separation was achieved on a CAPCELL PAK MG II C18 analytical column. Detection was performed using positive electrospray ion source in the multiple reaction monitoring mode. The method was fully validated for analyzing these principles in rat plasma with a lower limit of quantification from 0.5 to 5 ng/mL. The intra- and interbatch precisions were less than 10%, and the accuracies ranged from -7.5 to 8.0%. The extraction recovery of the analytes was above 70% without a significant matrix effect. The method was used to determine the oral and intravenous pharmacokinetic profiles of these furanocoumarins after dosing with Radix A. dahurica extract. The bioavailability of these furanocoumarins ranged from 10.1 to 82.8%. These data provide critical information for a better understanding of the pharmacological mechanisms and herb-drug interaction potential of Radix A. dahurica., (© 2015 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.)

The fruit of Psoralea corylifolia (Psoraleae Fructus) is a traditional Chinese medicine (TCM), which has been used to prevent and treat vitiligo, psoriasis, and osteoporosis in China for thousands of years. Phytochemical investigation on Psoraleae Fructus, as well as some metabolism research focused on pharmacokinetics of several single compounds from this plant, has been reported. However, the effective material of Psoraleae Fructus is still unknown. In the present study, the metabolic fate of multiple components of Psoraleae Fructus in rats was investigated by ultra performance liquid chromatography coupled with quadrupole time-of-flight tandem mass spectrometry (UPLC/Q-TOF-MS). Based on a three-step strategy, a total of 142 Psoraleae Fructus-related xenobiotics were identified or tentatively characterized in rat biofluids after oral administration of six representative single compounds and Psoraleae Fructus extract. All six different types of constituents of Psoraleae Fructus, including furocoumarin, coumestan, isoflavone, flavanone, chalcone and monoterpene phenol, could be absorbed into the circulation system. In addition, compared with the metabolism of six representative single compounds, different metabolic fate was observed after oral administration of Psoraleae Fructus extract, which indicated that the drug-drug interactions occurred when fed by multi-component herbal extract, and the investigations only focused on several main components were not sufficient to represent and reflect the overall efficacy of plants. The present study will be conducive to further pharmacological mechanism research on Psoraleae Fructus., (Copyright © 2015 Elsevier B.V. All rights reserved.)

Clausena lansium Skeels, a member of the Rutaceae, is a shrub or small tree with grapelike fruits. Several parts of this plant have been used in folk medicine. A bioactive constituent investigation of the stems of C. lansium herein resulted in isolation of four furanocoumarins, claucoumarins A-D, and 13 known analogs. Their structures were elucidated on the basis of spectroscopic analyses, including UV, IR, MS, and NMR experiments, and their absolute configurations were determined by CD experiments. Using an in vitro system, several of these compounds showed selective neuroprotective effects at a concentration of 10μM., (Copyright © 2014 Elsevier Ltd. All rights reserved.)

Introduction: The root of Angelica dahurica is a traditional Chinese medicine that used for the treatment of headache, toothache, abscess, furunculosis and acne. Coumarins were the major bioactive constituents of A. dahurica, hence it is worthwhile developing a method to simultaneously characterise them, especially those in trace amounts., Objective: To develop an efficient method for the simultaneous characterisation of coumarins in A. dahurica., Methods: A method using off-line two-dimensional high-performance liquid chromatography coupled with electrospray tandem mass spectrometry (off-line 2D-HPLC-ESI/MS(n) ) was developed., Results: In total 50 coumarins, including 32 linear furanocoumarins, 16 bifuranocoumarins and two non-furanocoumarins, were identified from the roots of A. dahurica. The possible MS fragmentations of these coumarins are also proposed., Conclusion: The method described here allows rapid and convenient identification of the coumarins in A. dahurica, and may be applied to other herbal medicines containing linear furanocoumarins., (Copyright © 2014 John Wiley & Sons, Ltd.)

A sensitive and specific high-performance liquid chromatography (HPLC) method was developed and applied to the pharmacokinetics for simultaneous identification and quantification of four components - puerarin, daidzein, imperatorin and isoimperatorin - in the plasma and tissues of normal and middle cerebral artery occlusion rats after oral administration of Baige capsule. Ferulic was used as the internal standard. The extraction procedure was composed of two independent steps. The plasma was prepared by liquid-liquid extraction with light petroleum-acetic ether (1:1, v/v) first and then protein was precipitated with methanol. The tissue samples were weighted and homogenated with normal saline, then the homogenate was prepared by liquid-liquid extraction and protein precipitation. The parameters of pharmacokinetics were calculated using DAS 2.1.1 software. The calibration curves of all four components in the plasma and tissue homogenates were in good linearity in the measured range with R(2)  ≥ 0.9921. The relative standard deviation of the intra- and inter-day accuracy at different levels was less than ±18.0%. In conclusion, the established method was a simple and effective one to simultaneously detect all four components in the plasma and tissues of rats, and was successfully applied in the pharmacokinetics of Baige capsule., (Copyright © 2013 John Wiley & Sons, Ltd.)

Objective: To investigate the chemical constituents in the roots of Angelica nitida., Methods: The chemical constituents were isolated by silica gel,their structures were identified by spectral analysis., Results: Nine compounds were isolated and identified as isoimperatorin(I), imperatorin(II), cnidilin(III), beta-sitosterol(IV), isopimpinellin(V), phellopterin(VI), neobyakangelicol(VII), (3S)-2,2-dimethyl-3,5-dihydroxy-8-hydroxylmethyl-3,4-dihydro-2H,6H-benzo[1,2-b: 5,4-b'] dipyran-6-one(VIll) and byakangelicin (IX)., Conclusion: All the compounds are isolated from the plant for the first time.

Aim: To examine the efficacy of YuanHu painkillers (YHP) as a treatment for primary dysmenorrhea and to reveal YHP's principle formula., Methods: A Wistar rat uterine contraction model was utilized in this study. Rats were given 0.698g/kg YHP, 0.07g/kg tetrahydropalmatine (THP; YHP's main component), 0.02g/kg imperatorin (IMP), or THP+IMP (0.07+0.02g/kg) as polypharmacy (PG) by gavage. H&E staining and histopathological examination of the uteri tissue samples were performed. We then detected superoxide dismutase (SOD) and malondialdehyde (MDA), nitric oxide (NO), as well as inducible nitric oxide synthase (iNOS), i-κB, nuclear factor-κB (NF-κB), and cyclooxygenase-2 (COX-2) indices., Results: PG significantly inhibited the uterine contraction of the primary dysmenorrhea rat model (p<0.05), and was significantly different than single-agent therapy (p<0.05). Histopathological examination showed inflammation in the uteri of the control group which YHP and its main constitutes alleviated. THP significantly inhibited the contraction of isolated uteri caused by Ach, PGF2α and oxytocin in a concentration-dependent fashion. THP and IMP both significantly affected the levels of NO, activation of NF-κB, up-regulated the expression of i-κB and down-regulated the expression of both iNOS and COX-2. IMP obviously decreased the level of MDA and increased the activation of SOD (p<0.05). PG obviously improved all the parameters mentioned above (p<0.05)., Conclusions: YHP exerted protective effects on primary dysmenorrhea in rats and remarkably alleviated the severity of experimental primary dysmenorrhea. The combined strategy proved to be more effective than either THP or IMP alone and may have synergistic effects in combination in primary dysmenorrhea. Mechanisms that might account for the beneficial effects include abating oxidative stress, inhibiting over-inflammatory reaction, and alleviating the contraction of isolated rat uteri by inhibiting the influx of extracellular Ca(2+). Broad potential for future clinical practice is foreseeable., (Copyright © 2013 Elsevier GmbH. All rights reserved.)

Imperatorin (IMP) is a major constituent of many herbal medicines and possesses anti-osteoporosis activity. The present research work aimed to study the biotransformation processes of IMP and evaluated the anti-osteoporosis activity of the transformed metabolites. Among 18 strains of filamentous fungi screened, Penicillium janthinellum AS 3.510 exhibited good capability to metabolise IMP to the new derivatives. Ten transformed products were isolated and purified, and their structures were identified accurately based on spectroscopic data. Eight metabolites (2-8 and 10) were novel and previously unreported. The major biotransformation reactions involved hydroxylation of the prenyloxy side-chain and the lactone ring-opening reaction of furocoumarin skeleton. In addition, anti-osteoporosis activities of all products (1-10) were evaluated using MC3T3-E1 cells. The results showed that products 5 and 8 had the best bioactivities in increasing MC3T3-E1 cell growth. These products could be used in future therapeutic regimens for treating osteoporosis., (Copyright © 2012 Elsevier Ltd. All rights reserved.)

Bioassay directed isolation of the EtOAc extract from a traditional Chinese medicine Psoralea corylifolia resulted in the purification of two isoflavonoids, corylifols D (1) and E (2), along with four known ones. The structures of 1 and 2 were determined by extensive 1D and 2D NMR and MS data analyses. When tested against HepG2 and Hep3B hepatocellular carcinoma cell lines, corylifol A (4) displayed IC50 values of 4.6 and 13.5 μg/ml, respectively.

In this study, 2 metabolites of imperatorin, imperatorin hydroxylate (IMH) and imperatorin epoxide (IME), were identified for the first time in dog plasma. A sensitive, specific, and accurate high-performance liquid chromatography-tandem mass spectrometry (LC-MS/MS) method was then developed for the simultaneous quantification of imperatorin and its 2 metabolites in dog plasma. Separation was achieved on an Agilent ZORBAX Extend-C(18) column (2.1 mm × 50 mm, 3.5 μm) at 30 °C. The mobile phase consisted of 0.02% ammonium acetate solution-methanol with a gradient program at a flow rate of 0.3 mL/min. Detection was performed using an electrospray ionization source operating in positive ion multiple reaction monitoring mode and by monitoring the ion transitions from 271 to 203 m/z for imperatorin, 309.4-224.1 m/z for IMH, 287-203 m/z for IME, and 441.3-325.2 m/z for simvastatin (the internal standard). Good linearity was shown over the concentration range of 1-500 ng/mL for imperatorin, and 0.2-500 ng/mL for IMH and IME. The validated method was successfully applied to a pharmacokinetic study of imperatorin in beagle dogs. The pharmacokinetic profiles of imperatorin and its 2 metabolites showed sex differences after the i.v. administration of imperatorin at a dose of 5 mg/kg., (Copyright © 2012 Elsevier B.V. All rights reserved.)

Objective: To study the chemical constituents of the root of Angelica dahurica cv. Qibaizhi., Method: The compounds were isolated and purified by the methods of solvent extraction and chromatographic technique, and their structures were identified on the basis of the analyses of spectral data., Result: Twenty-seven compounds were obtained and identified as isoimperatorin (1), alloisoimperatorin (2), oxypeucedanin hydrate (3), byakangelicin (4), alloimperatorin (5), beta-sitosterol (6), dibutylphthalate (7), 6-(3,3-dimethylallyloxy) -7-hydroxycoumarin {7-hydroxy-6-[ (3-methyl-2-butenyl) oxy] -coumarin, 8}, xanthotoxol (9), 5-hydroxy-8-methoxypsoralen ( 5-hydroxyxanthotoxin, 10), smyrindiol (11), umbelliferone (12), bergapten (13), imperatorin (14), phellopterin (15), isoimpinellin (16), 6-acyl-7-methoxycoumarin (17), psoralen (18), isoscopletin (19), scoparone (20), xanthotoxin (21), angelol A (22), oxypeucedanin ethanolate (oxypeucedanin hydrate-3"-ethyl ether, 23), dehydrogeijerin (pablohopin, 24) , ulopterol (25), heraclenol (26), and pabulenol (27), respectively., Conclusion: Compound 8 was a new natural product and the above-mentioned all the compounds except for compounds 1, 3 and 14 were isolated from the root of A. dahurica cv. Qibaizhi for the first time.

Objective: To develop a quantitative analysis of multi-components by single marker(QAMS) method for simultaneous determination of three coumarins in Angelica dahurica var. formosana, by using one standard substance., Method: With imperatorin as internal reference standard, and 2 relative correction factors (RCF) to imperatorin were calculated within certain ranges. Their contents in 20 batches of samples, collected from different areas, were determined by both external standard method and QAMS. The method was evaluated by comparison of the quantitative results between the two methods., Result: No significant differences were found in the quantitative results of three coumarins in 20 batches of A. dahurica var. formosana determined by the two methods (RSD < 5%)., Conclusion: QAMS is feasible and suitable for quality control of A. dahurica var. formosana.

Objective: To establish the HPLC fingerprint of Angelica polymorpha., Method: The 10 batches of A. polymorpha were measured by HPLC with isoimperatorin as a reference substance and the chromatographic experients were performed on Kromasil 100A C18 column (4.6 mm x 250 mm, 5 microm), eluted with acetonitrile and water as mobile phase in gradient mode. The flow rate was 1.0 m x min(-1) and the detection wavelength was 254 nm., Result: The common mode of the HPLC fingerprints were set up. There were 8 common peaks in the fingerprint of 10 samples, and the similarity of the 10 samples was more than 0.9., Conclusion: The method is simple, accurate and have a good reaptability. The quality of A. polymorpha can be controlled effectively by the HPLC fingerprint.

A high-performance liquid chromatography coupled with photo diode array detection method is developed for simultaneous determination of seven active components in Qibaomeiran pill, including rutin, 2,3,5,4'-tetrahydroxystilbene-2-O-beta-D-glycoside, ferulic acid, psoralen, isopsoralen, emodin, and physcion. The analysis is performed on a C(18) column using a mobile phase composed of A (0.1% acetic acid) and B (acetonitrile) with linear gradient elution. Four wavelengths at 245, 290, 320, and 350 nm were chosen as the monitoring wavelength to determine seven active components, respectively. All the compounds show good linearity (r > 0.999). The developed method is fully validated in respect to precision, repeatability, and accuracy. The proposed method is successfully applied to quantify the seven active components in different Qibaomeiran pill samples. The results indicate that the developed assay could be considered as a suitable quality control method for the Qibaomeiran pill.

Objective: To optimize the extraction technology for Psoralea corylifolia and Salvia miltiorrhiza., Method: An orthogonal test was adopted in this study. The contents of Tanshinone IIA, Salvianolic acid B, Psoralen and Isopsoralen were used as indices of appraisal. Data processing was carried out with the multiple guidelines grading method for optimizing the extraction condition., Result: The best extraction technology was to extract for 2 times with 8 fold ethanol solution (70%) and 1.5 h each time., Conclusion: The optimized extraction technology was rational and the extraction rate of the active principles is high.

Objective: To improve the processing method of Psoralea corylifolia., Methods: The self-made processing machine was used to flatten Psoralea corylifolia. Then it was extracted with water soluble and alcohol soluble with Psoralea corylifolia unflatten as the amount of Psoralea corylifolia and the content of psoralen and isopsoralen were factors. HPLC was used. The analytical column was a Supelco ODS-C18. The mobile phase consisted of methanol-water (43:57). The detector wavelength was 246 nm. The column temperature was 30 degrees C., Results: Under the same condition, the conditioning treatment increased the water or ethanol extracting amount of Psoralea corylifolia and the content of psoralen and isopsoralen of the processing samples compared with the unconditioning treatment. The amount of water soluble extracts and erhanol soluble extracts increased 0.61 times and 1.53 times, respectively. And the content of psoralen and isopsoralen in water soluble and erhanol soluble extracts increased 1.22 times., Conclusion: The method to flatten Psoralea corylifolia can significantly improve the content of extraction and extraction rate of active components. It can also enhance the clinical effectiveness. The method is reasonable and deserves to be popularized.

The main pharmacological constituents of Chinese traditional medicine herb Cnidium monnieri are coumarin compounds and volatile oil. In addition, it contains monoterpene polyols, glucides, as well as recently discovered sesquiterpene components. In recent years, rather active investigations of its anti-tumor were performed at home and abroad. C. monnieri possesses multi-aspect and comprehensive anti-tumor functions, involving directly tumor-inhibitory activity, anti-mutagenicity, reversing multi-drug tolerance of tumor, as well as improving immune functions and so on. In this review, chemical constituents, anti-tumor activities and relevant investigations of Fructus Cnidii were summarized recent decade.

Objective: To develop a method for the determination of columbianetin, columbianetin acetate and osthol in Angelica pubescens f. biserrata, Method: HPLC method, ODS column (6.0 mm x 150 mm) with a mobile phase of methanol-acetonitrile-0.025 mol.L-1 phosphoric acid (32:20:48), and wave length detection at 320 nm., Result and Conclusion: The method can be used for the quality control of raw medicinal materials.