praeruptorin-c and anomalin

Peucedani Radix is a popular traditional Chinese medicine herb with a long history in China. Praeruptorin A (PA), praeruptorin B (PB), and praeruptorin E (PE) are usually taken as important quality indexes of Peucedani Radix.. To establish a rapid method for simultaneous determination of PA, PB, PE, and moisture contents in Peucedani Radix using near-infrared (NIR) spectroscopy and chemometrics.. One hundred twenty Peucedani Radix samples were analyzed with HPLC as a reference method. The NIR spectral scanning range was from 12000 cm-1 to 4000 cm-1. Partial least squares (PLS) regression algorithm was used to establish calibration models. Three variable selection methods were investigated, including variable importance in projection (VIP), competitive adaptive reweighted sampling (CARS), and Monte Carlo uninformative variable elimination (MCUVE). The performances of the established models were evaluated by root-mean-square error (RMSEC) and determination coefficient (Rc2) of calibration set, root-mean-square error (RMSEP) and determination coefficient (Rp2) of prediction set, and residual predictive deviation (RPD).. A clear ranking of the performance of the calibration models could be as follows: CARS-PLS > MCUVE-PLS > VIP-PLS > Full-PLS. For CARS-PLS, Rp2, RMSEP, and RPD of the prediction set are as follows: 0.9204, 0.0860%, and 3.5850 for PA; 0.8011, 0.0431%, and 2.0868 for PB; 0.8043, 0.0367%, and 2.1569 for PE; and 0.9249, 0.3350%, and 3.6551 for moisture, respectively.. The NIR spectroscopy combined with CARS-PLS calibration models could be used for rapid and accurate determination of PA, PB, PE, and moisture contents in Peucedani Radix samples.

Topics: China; Coumarins; Spectroscopy, Near-Infrared

Praeruptorin A, B and C are major bioactive constituents in Peucedani Radix. They display anti-inflammatory effect, anti-hypertension effect, antiplatelet aggregation, potential anti-cancer activities and so on. They are worthy of investigation as potentially novel and versatile drugs.. To develop a method using micellar electrokinetic chromatography (MEKC) for the application in simultaneously separation and determination of praeruptorin A, B and C from Peucedani Radix and its medicinal preparations.. Method optimisation was carried out by investigating influences of significant factors on the separation. The method was subjected to validation. The determination of praeruptorin A, B and C in Peucedani Radix and its drug formulations was accomplished by the developed method.. The optimal separation condition was 20 mM borate buffer containing 40 mM sodium cholate (SC), 22 mM sodium dodecyl sulphate (SDS) and 25% (v/v) acetonitrile (pH 10.00); 15 kV of voltage; 25°C of temperature; detection at 224 nm. Under this condition, three analytes were baseline separated within 16 min. A good linearity was obtained with correlation coefficients from 0.9988 to 0.9995. The limits of detection (LODs) and limits of quantitation (LOQs) ranged from 0.50 to 0.80 μg/mL and from 1.50 to 2.50 μg/mL, respectively. The recoveries ranged between 95.3% and 103.4%.. The proposed method has been successfully applied to the simultaneous determination of praeruptorin A, B and C in Peucedani Radix and its pharmaceutical preparations. Additionally, it could be a potential alternative to the quality control of Peucedani Radix.

Topics: Buffers; Calibration; Chromatography, Micellar Electrokinetic Capillary; Coumarins; Hydrogen-Ion Concentration; Limit of Detection; Medicine, Chinese Traditional; Micelles; Reproducibility of Results; Sodium Cholate; Sodium Dodecyl Sulfate

Many chiral drugs are used as the racemic mixtures in clinical practice. The occurrence of enantioselectively pharmacological activities calls for the development of enantiospecific analytical approaches during pharmacokinetic studies of enantiomers. Sample preparation plays a key role during quantitative analysis of biological samples. In current study, a rapid and reliable online solid phase extraction-chiral high performance liquid chromatography-tandem mass spectrometry (online SPE-chiral LC-MS/MS) method was developed for the simultaneously enantiospecific quantitation of (+)-trans-khellactone (dTK), (+/-)-cis-khellactone (d/lCK), (+/-)-praeruptorin A (d/lPA), (+/-)-praeruptorin B (d/lPB) and (+)-praeruptorin E (dPE), the main active angular-type pyranocoumarins (APs) in Peucedani Radix (Chinese name: Qian-hu) or the major metabolites of those APs, in rat plasma. The validation assay results described here show good selectivity and enantiospecificity, extraction efficiency, accuracy and precision with quantification limits (LOQs) of 2.57, 1.28, 1.28, 1.88, 4.16, 4.16 and 4.18ngmL(-1) for dTK, lCK, dCK, dPA, dPB, lPB and dPE, respectively, while lPA was not detected in rat plasma due to the carboxylesterase(s)-mediated hydrolysis. In addition, the validated system was satisfactorily applied to characterize the pharmacokinetic properties of those components in normal and chronic obstructive pulmonary disease (COPD) rats following oral administration of Qian-hu extract. dCK and lCK were observed as the main herb-related compounds in plasma. Enantioselectively pharmacokinetic profiles occurred for dCK vs lCK, dPA vs lPA, and dPB vs lPB in either normal or COPD rats. The proposed whole system is expected to be a preferable analytical tool for in vivo study of chiral drugs, in particular for the characterization of enantioselectively pharmacokinetic profiles.

Topics: Administration, Oral; Animals; Calibration; Chromatography, High Pressure Liquid; Coumarins; Disease Models, Animal; Hydrolysis; Linear Models; Male; Pulmonary Disease, Chronic Obstructive; Rats; Rats, Wistar; Reproducibility of Results; Stereoisomerism; Tandem Mass Spectrometry

Peucedani Radix is a Chinese medicinal herb noted for its effects on treatments of respiratory and pulmonary disorders. As a part of a systematic pharmacokinetic evaluation of the herb in our laboratory, the present study investigated, for the first time, the metabolic profile of (+)-praeruptorin B (dPB) and (+)-praeruptorin E (dPE), two main bioactive constituents of Peucedani Radix in pooled liver microsomes of rats (RLMs) and humans (HLMs). dPE was eliminated faster than dPB in both species. The incubation of dPB with RLMs and HLMs resulted in eight (B1-B8) and nine (B1-B9) metabolites, respectively, while both RLMs and HLMs converted dPE into 13 metabolites (E1-13). Structures of all the metabolites were proposed through comparing their mass data obtained via tandem mass spectrometry on an MSD ion trap system (IT-MS/MS) coupled with high-resolution mass measurement by time-of-flight mass spectrometry (TOF-MS) with those of the respective parent compound. B1 and E1 were unambiguously identified as (-)-cis-khellactone. The formations of all the metabolites were NADPH-dependent. Oxidation and hydrolysis were demonstrated to be two predominant metabolic pathways of dPB and dPE. Oxidation initiated at either the C-3' or C-4' substituent, while hydrolysis only started from the C-3' substituent. Fragmentation of all metabolites followed similar pathways to those of the parent pyranocoumarins. The information on metabolic properties of dPB and dPE and the mass fragmentation profiles of their metabolites obtained in the present study will aid in characterization of metabolic profiles of other angular-type pyranocoumarins and further investigation of in vivo fates of these pyranocoumarins and the herb.

Topics: Animals; Apiaceae; Chromatography, Liquid; Coumarins; Drugs, Chinese Herbal; Humans; Male; Metabolic Networks and Pathways; Microsomes, Liver; Rats; Rats, Sprague-Dawley; Tandem Mass Spectrometry