Development and Validation of RP-HPLC Method for Vicenin-2, Orientin, Cynaroside, Betulinic Acid, Genistein, and Major 8 Bioactive Constituents with LC-ESI-MS/MS profiling in Ocimum genus

Author(s):  
Aboli Girme ◽  
Prajkta Bhoj ◽  
Ganesh Saste ◽  
Sandeep Pawar ◽  
Amit Mirgal ◽  
...  

Abstract Background Ocimum genus known as Tulsi or Basil is a prominent botanical class in Asian culture, especially in India. The leaves have an immunomodulatory, antioxidant, stress-relieving, and adaptogenic role in traditional and modern medicine, with prominent usage in herbal teas and nutraceuticals. Objective The HPLC-PDA method was developed and validated for vicenin-2, orientin, cynaroside, betulinic acid, genistein, with syringic acid, rosmarinic acid, eugenol, carnosic acid, oleanolic acid, ursolic acid, luteolin, apigenin for quantification and confirmed using a novel ESI -MS/MS method in the Ocimum samples. Method The methodology parameters were developed on the RP-C18 column with a gradient elution of 1 mL/min flow rate for 0.1% o-phosphoric acid and acetonitrile at 210 and 340 nm wavelengths. Result The validation data for 13 bioactive compounds showed good linearity (r2> 0.99) with sensitive LOD (0.034-0.684 µg/mL) and LOQ (0.100-2.068 µg/mL) with recoveries (83.66-101.53%).The results were found precise (RSD,<5.0%) and accurate (RE, -0.60-1.06) for the quantification. The method performance was verified and found robust by analyzing ten samples of O. tenuiflorum from the ten geographical states of India (RSD, < 5.0%). Conclusion The validated HPLC-PDA method was found selective and suitable for analyzing thirteen compounds in O. tenuiflorum and twelve cultivars from the Ocimum genus as a quality control tool. This method can be used in routine analysis as an inexpensive alternative to advanced techniques. Highlights This work is the first to report for vicenin-2, orientin, cynaroside, betulinic acid, and genistein, with simultaneous analysis of eight bioactive compounds in the Ocimum genus.

2017 ◽  
Vol 2017 ◽  
pp. 1-12 ◽  
Author(s):  
Vita Giaccone ◽  
Giuseppe Polizzotto ◽  
Andrea Macaluso ◽  
Gaetano Cammilleri ◽  
Vincenzo Ferrantelli

The aim of our present work was the development of a rapid high-performance liquid chromatography method with electrospray ionization and tandem mass spectrometry detection (LC-ESI-MS/MS) for the determination of several corticosteroids in cosmetic products. Corticosteroids are suspected to be illegally added in cosmetic preparations in order to enhance the curative effect against some skin diseases. Sample preparation step consists in a single extraction with acetonitrile followed by centrifugation and filtration. The compounds were separated by reversed-phase chromatography with water and acetonitrile (both with 0.1% formic acid) gradient elution and detected by ESI-MS positive and negative ionization mode. The method was validated at the validation level of 0.1 mg kg−1. Linearity was studied in the 5–250 μg L−1 range and linear coefficients (r2) were all over 0.99. The accuracy and precision of the method were satisfactory. The LOD ranged from 0.085 to 0.109 mg kg−1 and the LOQ from 0.102 to 0.121 mg kg−1. Mean recoveries for all the analytes were within the range 91.9–99.2%. The developed method is sensitive and useful for detection, quantification, and confirmation of these corticosteroids in cosmetic preparations and can be applied in the analysis of the suspected samples under investigation.


2008 ◽  
Vol 78 (6) ◽  
pp. 293-298 ◽  
Author(s):  
Bernhard Watzl

Inflammation is a pathological condition underlying a number of diseases including cardiovascular diseases, cancer, and chronic inflammatory diseases. In addition, healthy, obese subjects also express markers of inflammation in their blood. Diet provides a variety of nutrients as well as non-nutritive bioactive constituents which modulate immunomodulatory and inflammatory processes. Epidemiological data suggest that dietary patterns strongly affect inflammatory processes. Primarily the intake of fruit and vegetables as well as of whole wheat is inversely associated with the risk of inflammation. In addition to observational studies there are also data from human intervention studies suggesting an anti-inflammatory potential of these plant foods. At the level of bioactive compounds occurring in plant foods, primarily carotenoids and flavonoids seem to modulate inflammatory as well as immunological processes. In conclusion, there is convincing evidence that plant foods and non-nutritive constituents associated with these foods modulate immunological and inflammatory processes. By means of anti-inflammatory activities a plant-based diet may contribute to the lower risk of cardiovascular diseases and cancer. A high intake of vegetables, fruit, and whole wheat as recommended by all international nutrition authorities provides a wide spectrum of bioactive compounds at health-promoting concentrations.


Author(s):  
Jinglong Wang ◽  
Dandan Zheng ◽  
Nan Xu ◽  
Chao Zhang ◽  
Yingzi Wang ◽  
...  

AbstractTo realize the attribution and identification of absorbed components in rat serum after oral administration of Erhuang decoction prepared by semi-bionic enzyme extraction method, the fingerprints of serum samples were established using a HPLC-DAD-ESI-MS method. Thirty-two peaks in Erhuang decoction and 24 peaks in rat serum after oral administration of Erhuang decoction were detected. Among the 24 peaks detected in rat serum, 25 compounds were identified by comparing the retention time and mass spectrometry data with that of reference compounds, or by mass spectrometry analysis and retrieving the reference literatures. Among the identified 25 compounds in vivo, 24 were the original form of compounds absorbed from the detected compounds in vitro, and one was the metabolite compounds of licorice. By analyzing the mass spectrometry or ultraviolet absorption characteristics, other unidentified compounds in vivo were deduced to be the endogenous metabolites in serum or the original form and metabolites of the compounds existed in vivo. Results indicated that HPLC-DAD-ESI-MS is suitable for identifying the bioactive constituents in serum after oral administration of Erhuang decoction, and the findings would be beneficial to further research and development of the pharmacodynamic substance base of Erhuang decoction.


Plants ◽  
2021 ◽  
Vol 10 (10) ◽  
pp. 2218
Author(s):  
Irene Sánchez-Gavilán ◽  
Esteban Ramírez Chueca ◽  
Vicenta de la Fuente García

(1) Background: this study describes bioactive compounds in the following halophytes: Sarcocornia (S. alpini, S. pruinosa, and S. perennis) and Arthrocnemum (A. macrostachyum). The material comes from: coastal marshes in Tinto River, Guadiana River, and some interior provinces from the Iberian Peninsula. (2) Methods: the techniques used were Folin–Ciocalteu, GC-MS, and ESI-MS/MS. (3) Results: Five phenolic acids were found in Sarcocornia: trans-cinnamic, salicylic, veratric, coumaric, and caffeic acids. In addition, in Arthronemum, ferulic acid was also detected. The obtained flavonoids were cyanidin-3-O-arabinoside, luteolin-7-glucoside, dihydroquercetin, and p-coumaroyl-glucoside. They also presented fatty acids, such as palmitic, linoleic, and oleic acids in Sarcocornia, while palmitic, linolenic, and stearic acids were the main fatty acids in A. macrostachyum. (4) Conclusions: the high diversity of the compounds identified confirms the relation between nutritional interest and salt tolerance in halophytes.


Phytomedicine ◽  
2014 ◽  
Vol 21 (4) ◽  
pp. 551-559 ◽  
Author(s):  
Xiaoyan Wu ◽  
Yuan Zhou ◽  
Fangzhou Yin ◽  
Chunqin Mao ◽  
Lin Li ◽  
...  

2020 ◽  
Vol 32 (5) ◽  
pp. 1183-1190
Author(s):  
K. Durga Raja ◽  
V. Saradhi Venkata Ramana ◽  
K. Raghu Babu ◽  
B. Kishore Babu ◽  
V. Jagadeesh Kumar ◽  
...  

Development and validation of six potential impurities by ultra performance liquid chromatography electro spray ionization tandem mass (UPLC-ESI-MS/MS) method for dronedarone hydrochloride drug was accomplished coherent with ICH guidelines. Successful chromatographic separation of dronedarone with its six impurities was attained by using gradient elution mode on RP-UPLC column using three pump mode system of 0.1 % formic acid in water as mobile phase A, methanol as the mobile phase B and solvent mixture of methanol, acetonitrile and water in the ratio of 65:30:5 v/v/v as the mobile phase C. Chromatographic conditions were set as 0.3 mL min-1 flow rate at the column temperature of 45 °C with the injection volume 2 μL. Briefly, the method enabled quantitation of six impurities with high accuracy (recovery > 90 %) and precision (% RSD < 5.0),within the ranges of 0.18-2.82 μg g-1. The regression (r) for each impurity over a range was > 0.99. The detection limit and quantitation limit of impurities were set at 0.09 and 0.18 μg g-1, respectively. The performed validation tests proved the suitability of the method for its intended purposes.


Molecules ◽  
2019 ◽  
Vol 24 (19) ◽  
pp. 3511 ◽  
Author(s):  
Federica Corana ◽  
Valentina Cesaroni ◽  
Barbara Mannucci ◽  
Rebecca Michela Baiguera ◽  
Anna Maria Picco ◽  
...  

Hericium erinaceus is a medicinal mushroom that contains many molecules promising a plethora of therapeutic properties. In this study, the strain H.e.2 (MicUNIPV, University of Pavia, Italy) was isolated from a sporophore collected in Tuscany (Italy). Mycelium, primordium, and wild type and cultivated sporophores were analyzed by HPLC-UV-ESI/MS. Erinacine A in the mycelium and hericenones C and D in the sporophores were quantified by comparison with their standard molecules. For the first time, H. erinaceus primordium was also investigated for the presence of these molecules. Comparing with the literature data, hericenes, molecules structurally similar to hericenones, were present in all our samples. The highest contents of hericenones C and D were detected in cultivated sporophores, compared to the wild type. The comparison of these data with those of another Italian H. erinaceus strain (H.e.1 MicUNIPV) was discussed. The results led us to select H. erinaceus strains more suitable for mycelium production or sporophore cultivation to obtain extracts with a higher content of bioactive compounds. This work provides a further step towards standardizing the procedures in the development of dietary supplements made from mushrooms.


2020 ◽  
Vol 32 (7) ◽  
pp. 1733-1740
Author(s):  
K. Durga Raja ◽  
V. Saradhi Venkata Ramana ◽  
K. Raghu Babu ◽  
B. Kishore Babu ◽  
V. Jagadeesh Kumar ◽  
...  

The objective of this work was to develop and validate a rapid, highly sensitive ultra performance liquid chromatography-tandem mass spectrometry (UPLC-ESI-MS/MS) method for the quantification of 2-isopropyl-4-(chloromethyl)thiazole in ritonavir. Chromatographic conditions of this impurity were achieved on an AQUITY UPLC column HSS (high strength silica) T3 column (100 mm long, 2.1 mm internal diameter, 1.8 μm diameter) using a gradient elution with 0.1% formic acid in water and methanol at a flow rate of 0.3 mL/min. LCMS/MS was operated under the multiple reaction mode (MRM) using electrospray ionization technique in positive ion mode and the transitions of m/z 176.1[M+H]+→140.1 for quantifier, 176.1[M+H]+→71.0 for qualifier were used to measure the impurity, respectively. The total chromatographic run time was 10 min. Full validation of the analytical method was carried out, including its system precision, selectivity, linearity, accuracy, recovery, ruggedness, stability and robustness. A linear response function was achieved in the concentration range of 0.12-1.86 μg/g with r > 0.99. The detection limit and quantitation limit of this impurity were 0.06 and 0.12 μg/g, respectively. Consistent recoveries were obtained during intra- and inter-day precision experiments in validation ranged from 80-120%. The developed method could be helpful not only for quality control and also for risk management of potential genotoxicity of this impurity in ritonavir drug substance.


2020 ◽  
Vol 15 (6) ◽  
pp. 1934578X2093196
Author(s):  
An-ping Yang ◽  
Zhao-guang Zheng ◽  
Fang Liu ◽  
Jing Liu ◽  
Rui-xue Wang ◽  
...  

Prunellae Spica (PS), the dry spikes of Prunella vulgaris L., is a medicinal herb widely distributed in Asia and Europe. As a traditional Chinese medicine, PS has been used for the treatment of mastitis, infectious hepatitis, and hypertension. The oral solution and some compounds (polysaccharide, ursolic acid, and betulinic acid) of PS have been reported to show activities against breast cancer. In this study, Michigan Cancer Foundation-7 (MCF-7) cell extraction coupled with high-performance liquid chromatography-electrospray ionization-tandem mass spectrometry (HPLC-ESI-MS/MS) analysis was applied to screen for potential antibreast cancer ingredients from PS. Protocatechuic acid (1), protocatechualdehyde (2), caffeic acid (3), and rosmarinic acid (4) were identified as high-affinity components. The cytotoxic activities of these compounds were evaluated in MCF-7 cells using Cell Counting Kit-8 assay. All the compounds displayed cytotoxicity to MCF-7 cells, but protocatechualdehyde and caffeic acid exhibited significant cytotoxicity with half-maximal inhibitory concentration values of 10.9 μM and 26.8 μM, respectively. This study provides the first report of the successful usage of cell extraction coupled with LC-MS/MS to screen active ingredients from PS. This method can be used as a screening tool for bioactive constituents in natural products.


Sign in / Sign up

Export Citation Format

Share Document