Development and validation of a HPLC-UV-ESI-MS method for the simultaneous quantitation of ten bioactive compounds in Dahuang Fuzi Tang

2014 ◽  
Vol 12 (12) ◽  
pp. 952-960 ◽  
Author(s):  
Hui GUO ◽  
Huan LI ◽  
Xiao LIU ◽  
Hao CAI ◽  
Li WU ◽  
...  
2021 ◽  
Vol 22 (13) ◽  
pp. 6972
Author(s):  
Ilona Sadok ◽  
Katarzyna Jędruchniewicz ◽  
Karol Rawicz-Pruszyński ◽  
Magdalena Staniszewska

Metabolites and enzymes involved in the kynurenine pathway (KP) are highly promising targets for cancer treatment, including gastrointestinal tract diseases. Thus, accurate quantification of these compounds in body fluids becomes increasingly important. The aim of this study was the development and validation of the UHPLC-ESI-MS/MS methods for targeted quantification of biologically important KP substrates (tryptophan and nicotinamide) and metabolites(kynurenines) in samples of serum and peritoneal fluid from gastric cancer patients. The serum samples were simply pretreated with trichloroacetic acid to precipitate proteins. The peritoneal fluid was purified by solid-phase extraction before analysis. Validation was carried out for both matrices independently. Analysis of the samples from gastric cancer patients showed different accumulations of tryptophan and its metabolites in different biofluids of the same patient. The protocols will be used for the evaluation of tryptophan and kynurenines in blood and peritoneal fluid to determine correlation with the clinicopathological status of gastric cancer or the disease’s prognosis.


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.


2010 ◽  
Vol 43 (15) ◽  
pp. 2456-2464 ◽  
Author(s):  
Yong Chen ◽  
Yerui Li ◽  
Xueying Chen ◽  
Longhu Wang ◽  
Changhai Sun ◽  
...  

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.


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.


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