scholarly journals Development of validated UHPLC–PDA with ESI–MS-MS method for concurrent estimation of magnoflorine, berbamine, columbamine, jatrorrhizine, palmatine and berberine in Berberis aristata

Author(s):  
Ishita A. Basera ◽  
Aboli Girme ◽  
Vijay P. Bhatt ◽  
Ganesh Saste ◽  
Sandeep Pawar ◽  
...  

Abstract A validated UHPLC-PDA with an ESI-MS/MS method has been developed for simultaneous estimation of six bioactive alkaloids (magnoflorine, berbamine, columbamine, jatrorrhizine, palmatine and berberine) in the different extracts of the roots of Berberis aristata DC (Family:Berberdiaceae). It is an important medicinal herb native to Northern Himalaya and commonly known as ‘daruharidra’, ‘daruhaldi’, ‘Indian barberry’ or ‘tree turmeric’. An insight into the research literature uncovered reports on isoquinoline alkaloids like magnoflorine, berbamine, columbamine, jatrorrhizine, palmatine, and berberine as major bioactives in B. aristata roots, possessing different pharmacological and therapeutic effects. In the present study, these aforementioned alkaloids were separated on Phenomenex Luna®, 5 µm-C8 analytical column. The HPLC-MS analysis was performed at a flow rate of 0.90 mL min−1. Each alkaloid that is resolved was characterized by precursor ions and fragment ions with electrospray ionization (ESI) source in both positive and negative ionization using scan mode. The limit of detections (LODs) were 0.087, 0.727, 0.035, 0.124, 0.782 and 0.794 μg mL−1 for magnoflorine, berbamine, columbamine, jatrorrhizine, palmatine and berberine, respectively. The proposed UHPLC-PDA method was fully validated according to international (ICH) guidelines and was found to be selective, sensitive and highly accurate for the concomitant estimation of the aforementioned symbolic bio-markers of B. aristata roots.

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.


Author(s):  
Bhupender Tomar ◽  
Ankita Sharma ◽  
Inder Kumar ◽  
Sandeep Jain ◽  
Pallavi Ahirrao

A simple, precise, and accurate reverse phase high performance liquid chromatographic method (RP-HPLC) was developed and validated for the estimation of the combination of 5- Fluorouracil (5-FU) and Imiquimod in active pharmaceutical ingredients (APIs). The method was carried out on Phenomenex C18 (250 × 4.6mm I.D., 5𝜇m) using isocratic elution mode. The mobile phase was used as Acetonitrile: 10mM potassium dihydrogen orthophosphate: triethylamine (40:59.9:0.1, v/v, pH 4.5 with orthophosphoric acid) and Water: ACN (50:50 v/v) was used as a diluent. The concentration of solvents was 1-20µg/ml and the volume of injection was 20µl with the flow rate of 1.2ml/min. The retention times for 5-FU and Imiquimod were found to be 1.9±0.5 and 6.6±0.5 min respectively. The absorption maxima of 5FU and Imiquimod were found 267nm and 227nm respectively. The method was validated as per ICH guidelines. All the data were found within the specified limits. The limit of detection (LOD) and limit of quantification (LOQ) of 5- Fluorouracil were found to be 0.015μg/mL and 0.048 μg/mL, respectively, and Imiquimod was found to be 0.078μg/mL and 0.237μg/mL, respectively. The method developed in the present study was found to be sensitive, specific, and precise and can be applied for the simultaneous estimation of 5-FU and Imiquimod.


INDIAN DRUGS ◽  
2013 ◽  
Vol 50 (05) ◽  
pp. 36-43
Author(s):  
N. R Dighade ◽  
◽  
M. D Shende ◽  
A. V Kasture

A simple and accurate high performance thin layer chromatographic (HPLTC) method has been developed and validated as per ICH guidelines for estimations of Ciprofloxacin (CP) and Ornidazole (ORN) in combined dosage form. The mobile phase was acetonitrile: toluene: water and triethylamine (5.5:1.8:1.5:1.6 V/V) was found to be best which gave high resolution with Rf 0.16 and 0.84 for ciprofloxacin and ornidazole respectively. The linearity of ciprofloxacin and ornidazole was found to be in the range of 0.4 to 0.8 µg/mL and 0.4 to 0.8 µg/mL, respectively. The coefficient of correlation (r2 ) was found to be greater than 0.989 for both the components by this method. The tablet analyses result (n = 5) were found to be > 100.84 % by HPTLC for both the components. The proposed method was found to be simple, accurate and suitable for routine quality control of marketed formulations containing these drugs.


INDIAN DRUGS ◽  
2019 ◽  
Vol 56 (09) ◽  
pp. 43-54
Author(s):  
K Vijaya Sri ◽  
M. Madhuri ◽  
V. Anusha ◽  
V.R.K. Siresha ◽  

The present research work illustrates the development and validation of RP HPLC method for simultaneous estimation of tenofovir disproxil fumarate, emtricitabine and rilpivirine hydrochloride in bulk and formulated in a pharmaceutical dosage form as a nanosupension. Antiretroviral drug treatment is the primary line of therapy for treating HIV. The multicomponent system formulated as a nanosuspension evidenced increased hydrophilicity, potency and decreased side effects. The separation was carried out by using efficient BDS hypersil C18 HPLC column with empower software. Combination method of Precipitation—ultrasonic homogenization was used for the preparation of the nanosuspension. The mobile phase used was methanol, water, acetonitrile (80:13.4:6.6) v/v and flow rate 1mL /min. The developed method was thus validated as per ICH guidelines for various parameters whose results advocated the reliability of the method. The results for parameters viz. retention times of tenofovir disproxil fumarate, emtricitabine and rilpivirine were 3.09 min, 2.78 min and 3.68 min, linearity range was between 7.5-90, 5-60, 0.625-7.5µg/mL, respectively. Thus the new RP-HPLC method is optimum, reliable and can be used for the simultaneous estimation of tenofovir disproxil fumarate, emtricitabine and rilpivirine hydrochloride.


Author(s):  
Ruzimov Sanjarbek ◽  
Jamshid Mavlonov ◽  
Akmal Mukhitdinov

The paper aims to present an analysis of the component sizes of commercially available vehicles with electrified powertrains. The paper provides insight into how the powertrain components (an internal combustion engine, an electric motor and a battery) of mass production electrified vehicles are sized. The data of wide range of mass production electrified vehicles are collected and analyzed. Firstly, the main requirements to performance of a vehicle are described. The power values to meet the main performance requirements are calculated and compared to the real vehicle data. Based on the calculated values of the power requirements the minimum sizes of the powertrain components are derived. The paper highlights how the sizing methodologies, described in the research literature, are implemented in sizing the powertrain of the commercially available electrified vehicles.


INDIAN DRUGS ◽  
2015 ◽  
Vol 52 (02) ◽  
pp. 20-33
Author(s):  
N. S Kumar ◽  
◽  
R Kumaraswamy ◽  
S. Shantikumar ◽  
D. Paul

The present study describes the separation and simultaneous estimation of eight anti-retroviral drugs, namely, Telaprevir (TPV), Emtricitabine (ECB), Fosamprenavir (FANV), Tenofavir (TNF), Ritonavir (RNV), Raltegravir (RGV) and Oseltamivir (OSMV) and Zidovudine (ZDV) as an active pharmaceutical ingredient, by RP-HPLC method by applying the principles of Quality by Design (QbD). An application of DoE (Design of Experiments) full factorial design was used for initial screening and optimization. The final optimized method consists of separation being carried out on a Fortis C18 column (150 mm × 4.6 mm, 5μ particle size) using acetonitrile and 10 mm ammonium formate buffer (pH 3 adjusted with formic acid) using a gradient program. The quantitative evaluation was performed with a diode array detector at 251 nm and 230 nm with a flow rate of 1 mL min–1. Suitability of this method for the quantitative determination of the drugs was proved by validation in accordance with the International Conference on Harmonization (ICH) guidelines. The method is selective, precise, robust and accurate and can be used for routine analysis of pharmaceutical formulations in quality control and counterfeit screening.


2019 ◽  
Vol 27 (3) ◽  
pp. 393-410 ◽  
Author(s):  
Maria Bada ◽  
Jason R.C. Nurse

PurposeThe purpose of this study is to focus on organisation’s cybersecurity strategy and propose a high-level programme for cybersecurity education and awareness to be used when targeting small- and medium-sized enterprises/businesses (SMEs/SMBs) at a city-level. An essential component of an organisation’s cybersecurity strategy is building awareness and education of online threats and how to protect corporate data and services. This programme is based on existing research and provides a unique insight into an ongoing city-based project with similar aims.Design/methodology/approachTo structure this work, a scoping review was conducted of the literature in cybersecurity education and awareness, particularly for SMEs/SMBs. This theoretical analysis was complemented using a case study and reflecting on an ongoing, innovative programme that seeks to work with these businesses to significantly enhance their security posture. From these analyses, best practices and important lessons/recommendations to produce a high-level programme for cybersecurity education and awareness were recommended.FindingsWhile the literature can be informative at guiding education and awareness programmes, it may not always reach real-world programmes. However, existing programmes, such as the one explored in this study, have great potential, but there can be room for improvement. Knowledge from each of these areas can, and should, be combined to the benefit of the academic and practitioner communities.Originality/valueThe study contributes to current research through the outline of a high-level programme for cybersecurity education and awareness targeting SMEs/SMBs. Through this research, literature in this space was examined and insights into the advances and challenges faced by an on-going programme were presented. These analyses allow us to craft a proposal for a core programme that can assist in improving the security education, awareness and training that targets SMEs/SMBs.


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.


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