scholarly journals Preparation of Oxymel (Sekanjabin-e) Buzuri Syrup as Vascular Opener (Mofatteh) Product and Its Standardization

2020 ◽  
pp. 1-6
Author(s):  
Sima Sadrai ◽  
Maryam Yakhchali ◽  
Mehran Mirabzadeh Ardakani ◽  
Mahdi Alizadeh Vaghasloo ◽  
Mahdi Vazirian ◽  
...  
Keyword(s):  
Chlorogenic Acid ◽  
Cardiovascular Health ◽  
Gradient Elution ◽  
Reversed Phase ◽  
Hplc Method ◽  
Apium Graveolens ◽  
Marker Compound ◽  
Pimpinella Anisum ◽  
Complementary Product ◽  
Cuscuta Chinensis

Background: Sekanjabin-e buzuri consisting extracts of Chicorium intybus L. (Kasni), Cuscuta chinensis Lam. (Koshus), Apium graveolens L. (Karafs) and Pimpinella anisum L. (Anison) seeds is a Traditional Persian Medicine product. These drugs have many applications in traditional medicine, but they are more effective in opening vascular obstructions and related functions, especially in cardiovascular system. Purpose: In this study we prepared a proper Sekanjabin-e buzuri and developed a HPLC method for analysis of chlorogenic acid (CGA), as an herbal marker compound, for quality control and standardization in both Sekanjabin-e buzuri syrup and its ingredient sources. Methods: Sekanjabin-e buzuri is a group of oxymels that have many different formulations. A proper formulation has chosen from literature (from Gharabadin-e-salehi) and prepared. For standardization of Sekanjabin-e buzuri we developed a method for detecting chlorogenic acid content. A reversed phase MZ C18 column (150*3.0 mm, 5µm) using a mixture of acetonitrile-phosphoric acid 0.1% with gradient elution program for 20 minutes with flow rate of 1.5 ml/min with UV detection at 330 nm. Results: The chlorogenic acid Rt =5.1 minutes and linear over the range of 0.2-1.5 µg/ml, (R2 = 0.9996). The calculated LOD and LOQ of chlorogenic acid were 0.02 and 0.06 µg/ml, respectively. The concentration of chlorogenic acid was 7.69, 10.37, 2.25, 2.88 and 22.86 µg/ml for Chicorium intybus L., Cuscuta chinensis Lam., Apium graveolens L. and Pimpinella anisum L. seeds and Sekanjabin-e buzuri syrup, respectively. Conclusion: This standardized Sekanjabin-e buzuri syrup will be used as a vascular opener (Mofatteh) complementary product for opening internal organs obstruction e.g. promoting cardiovascular health.

scholarly journals Simultaneous determination of mycophenolic acid and its glucuronide in human plasma using a simple high-performance liquid chromatography procedure

1998 ◽  
Vol 44 (7) ◽  
pp. 1481-1488 ◽  
Author(s):  
Maria Shipkova ◽  
Paul Dieter Niedmann ◽  
Victor William Armstrong ◽  
Ekkehard Schütz ◽  
Eberhard Wieland ◽  
...  
Keyword(s):  
Mycophenolic Acid ◽  
High Performance ◽  
Internal Standard ◽  
Gradient Elution ◽  
Reversed Phase ◽  
Hplc Method ◽  
Free Concentration ◽  
Elution Chromatography ◽  
Glucuronide Metabolite

Abstract We describe a reversed-phase HPLC method for determination of total mycophenolic acid (MPA), its free concentration (MPAf), and the glucuronide metabolite (MPAG), based on simple sample preparation and gradient elution chromatography. The compounds were quantified in parallel by absorbance at 254 nm and 215 nm in the internal standard mode. Linearity was verified up to 50 mg/L for MPA and up to 500 mg/L for MPAG (r >0.999). Detection limits at 215 and 254 nm were, respectively, 0.01 and 0.03 mg/L for MPA, and 0.03 and 0.1 mg/L for MPAG. The recovery of MPA was 95–106%;recovery of MPAG was 96–106%. The imprecision (CV) for MPA (0.2–25 mg/L) was <8.4% (254 nm) and <4.4% (215 nm) within day (n = 12) and <9.2% (254 nm) and <6.2% (215 nm) between days (n = 12). The imprecision for MPAG (10–250 mg/L) was <4.9% (254 nm) and <3.4% (215 nm) within day, and <6.1% (254 nm) and <5.9% (215 nm) between days. For quantification of MPAf, 100 μL of ultrafiltrate was applied directly to the column. The detection limit was 0.005 mg/L at 215 nm and 0.015 mg/L at 254 nm. In the range between 18–210 μg/L, the within-day CVs were <11.8% (n = 12) and the between-day CVs were <15.8% (n = 12).

scholarly journals Simultaneous Determination of Eight Synthetic Permitted and Five Commonly Encountered Nonpermitted Food Colors in Various Food Matrixes by High-Performance Liquid Chromatography

2010 ◽  
Vol 93 (5) ◽  
pp. 1503-1514 ◽  
Author(s):  
Sumita Dixit ◽  
Subhash K Khanna ◽  
Mukul Das
Keyword(s):  
Simultaneous Determination ◽  
High Performance ◽  
High Sensitivity ◽  
Gradient Elution ◽  
Reversed Phase ◽  
Hplc Method ◽  
Food Category ◽  
Food Commodities ◽  
Food Colors

Abstract A simple and sensitive HPLC method has been developed for the simultaneous determination of eight permitted food colors and five commonly encountered nonpermitted colors in various food commodities, including sugar-, fat-, and starch-based food matrixes. The method uses a specific food category-based cleanup/treatment procedure before color extraction to avoid the interference of food matrixes, and to obtain the optimal color extraction. Analysis was performed on a reversed-phase C18 -Bondapak column with ammonium acetate and acetonitrile gradient elution as the mobile phase; a programmable max-specific visible detection was used to monitor colors to obtain the higher sensitivity and expanded scope needed for multicolor blends having diverse absorption maxima. All colors showed good linearity, with regression coefficients of 0.99740.9999. The LOD and LOQ values ranged from 0.01 to 0.12 mg/L, and from 0.04 to 0.83 mg/L or mg/kg, respectively. The intraday and interday precision tests produced good RSD values, and the recoveries from different food matrixes ranged from 82 to 104%. The method offers high sensitivity for analysis of a wide variety of food matrixes containing a broad scope of multicolor blends. Two nonpermitted colors, orange II and metanil yellow, were found. Also, a number of samples contained permitted colors at levels two-to seven-fold higher than those prescribed.

scholarly journals Rapid HPLC Measurement of Thiamine and Its Phosphate Esters in Whole Blood

2008 ◽  
Vol 54 (5) ◽  
pp. 901-906 ◽  
Author(s):  
Jun Lu ◽  
Elizabeth L Frank
Keyword(s):  
Whole Blood ◽  
Clinical Laboratory ◽  
Vitamin B1 ◽  
Current Method ◽  
Gradient Elution ◽  
Reversed Phase ◽  
Hplc Method ◽  
Phosphate Esters ◽  
Healthy Population ◽  
Limit Of Quantification

Abstract Background: Thiamine (vitamin B1) deficiency is associated with severe diseases such as beriberi and Wernicke encephalopathy. Although most Americans have sufficient dietary intake, thiamine deficiency is observed in the alcohol-dependent and elderly populations. Measurement of thiamine concentration in whole blood provides an assessment of vitamin B1 status in at-risk individuals. Method: We used TCA to precipitate proteins in whole blood. Thiamine and its phosphate esters were derivatized using potassium ferricyanide to thiochromes, which were separated by gradient elution on a reversed-phase HPLC column and detected by fluorescence. The method was validated for linearity, limit of quantification, imprecision, accuracy, and interference. Results obtained with this method were compared with those produced by the method currently used in our clinical laboratory. Reference values of thiamine and its phosphate esters were determined in samples obtained from self-reported healthy adults who were not taking vitamin supplements. To shorten analysis time, our method used whole blood rather than washed erythrocytes, did not require lengthy enzymatic dephosphorylation, and had a simple mobile phase. Results: The method was linear to 4000 nmol/L. The lower limit of quantification was 3 nmol/L. The within-run CV was <3.5% and total CV was <9.4%. This method correlated with our current method (r = 0.97). Approximately 90% of the total thiamine content in whole blood was present as thiamine diphosphate (TDP). The means (ranges) for an apparently healthy population were 114 (70–179) nmol/L for TDP and 125 (75–194) nmol/L for total thiamine. Results for separation and measurement of free thiamine and thiamine phosphate esters in whole blood were obtained within 5.5 min. Conclusion: We developed an HPLC method that allows separation and measurement of free thiamine and thiamine phosphate esters in whole blood and provides more rapid results than other methods.

scholarly journals A New Validated Stability indicating RP-HPLC Method for Simultaneous Quantification of Impurities of Fluticasone Propionate and Salmeterol Xenafoate in Metered Dose Inhalation Aerosol

2021 ◽  
Vol 33 (4) ◽  
pp. 867-872
Author(s):  
Surya Prakash Mamillapalli ◽  
Shirisha Koyya ◽  
B. Venkata Subbaiah ◽  
N. Annapurna
Keyword(s):  
Fluticasone Propionate ◽  
Drug Product ◽  
Gradient Elution ◽  
Reversed Phase ◽  
Hplc Method ◽  
Forced Degradation ◽  
Stability Indicating ◽  
Simultaneous Quantification ◽  
Metered Dose ◽  
Dose Inhalation

A simple, specific, precise, accurate and stability indicating reversed phase HPLC method for simultaneous quantification of total 12 impurities of fluticasone propionate and salmeterol xenafoate in metered dose inhalation aerosol has been developed in the present work. Chromatographic separation between impurities of both compounds were achieved on Altima C18 250 × 4.6 mm, 5 μ column using a step-gradient elution at a flow rate of 1.4 mL/min, 0.1% v/v orthophosphoric acid as buffer and acetonitrile as mobile phase constituents. Forced degradation studies for drug product were performed and revealed that Salmeterol is acid sensitive (about 21.3%), degrades to IMP-D and fluticasone is alkali sensitive (about 7.6%) and degrades to IMP-A. All degradant and process related impurities of both compounds were monitored at 214 nm and spectral purity along with % mass balance is assessed using PDA detector, which proved stability indicating capability of the method. The developed method is fully validated as per current ICH guidelines, where precision is achieved at % RSD of < 5, Correlation of < 0.999 for linearity, LOD-LOQ at < 0.02% and < 0.05%, along with satisfactory system suitability results under robustness conditions.

scholarly journals A Novel HPLC Method for the Concurrent Analysis and Quantitation of Seven Water-Soluble Vitamins in Biological Fluids (Plasma and Urine): A Validation Study and Application

2012 ◽  
Vol 2012 ◽  
pp. 1-8 ◽  
Author(s):  
Margherita Grotzkyj Giorgi ◽  
Kevin Howland ◽  
Colin Martin ◽  
Adrian B. Bonner
Keyword(s):  
Biological Fluids ◽  
Gradient Elution ◽  
Reversed Phase ◽  
Hplc Method ◽  
Water Soluble ◽  
Linear Gradient ◽  
Plasma And Urine Samples ◽  
Urine Separation ◽  
Concurrent Analysis ◽  
Alcohol Dependent

An HPLC method was developed and validated for the concurrent detection and quantitation of seven water-soluble vitamins (C, B1, B2, B5, B6, B9, B12) in biological matrices (plasma and urine). Separation was achieved at 30°C on a reversed-phase C18-A column using combined isocratic and linear gradient elution with a mobile phase consisting of 0.01% TFA aqueous and 100% methanol. Total run time was 35 minutes. Detection was performed with diode array set at 280 nm. Each vitamin was quantitatively determined at its maximum wavelength. Spectral comparison was used for peak identification in real samples (24 plasma and urine samples from abstinent alcohol-dependent males). Interday and intraday precision were <4% and <7%, respectively, for all vitamins. Recovery percentages ranged from 93% to 100%.

scholarly journals Standardization of Adhatoda vasica Nees Market Preparations by RP-HPLC Method

2016 ◽  
Vol 15 (1) ◽  
pp. 57-62 ◽  
Author(s):  
BK Sajeeb ◽  
Uttom Kumar ◽  
Md Shahadat Hossain ◽  
Sitesh C Bachar
Keyword(s):  
Mobile Phase ◽  
Reversed Phase ◽  
Hplc Method ◽  
Reversed Phase Hplc ◽  
Reference Standard ◽  
Adhatoda Vasica ◽  
Traditional Medicines ◽  
Marker Compound ◽  
Rp Hplc ◽  
Qualitative Analyses

In recent times, quality control of herbal and traditional medicines with modern scientific techniques and knowledge are of great concern. The present study reveals a simple and improved reversed phase HPLC method for qualitative analyses of Adhatoda vasica Nees market preparations via quantitation of its major metabolite, vasicine as a marker compound. Three market preparations, each of four different herbal and traditional manufacturers, were analyzed. The market preparations were extracted with chloroform and the residue obtained from extraction of each market preparation was analyzed for quantitation of vasicine by RP-HPLC method with ODS column using a mixture of water and methanol (60:40) as mobile phase at a flow rate of 0.5 ml/min. The estimated quantities of vasicine compared to reference standard for marketed products of four different manufacturers were found to be 1.502 ± 0.064 g, 1.590 ± 0.081 g, 1.761 ± 0.061 g and 1.627 ± 0.082 g, respectively per 100 ml of preparation.Dhaka Univ. J. Pharm. Sci. 15(1): 57-62, 2016 (June)

SIMULTANEOUS DETERMINATION OF DOMPERIDONE AND PARABEN PRESERVATIVE IN ORAL FORMULATION: REVERSED-PHASE LIQUID CHROMATOGRAPHIC METHOD

INDIAN DRUGS ◽  
2019 ◽  
Vol 56 (08) ◽  
pp. 81-83
Author(s):  
A Patel ◽  
S. D Firke ◽  
R. R. Patil ◽  
M. G. Kalaskar ◽  
S. B. Bari ◽  
...  
Keyword(s):  
Sodium Benzoate ◽  
Gradient Elution ◽  
Oral Formulation ◽  
Reversed Phase ◽  
Hplc Method ◽  
Oral Solution ◽  
Chromatographic Separations ◽  
Phase Liquid ◽  
Liquid Chromatographic

A novel RP-HPLC method was developed and validated for the determination of compounds in an oral solution. The method describes the determination of domperidone along with sodium methylparaben, sodium propylparaben and sodium benzoate in liquid oral formulation. The chromatographic separations were performed using BDS Hypersil 5 μm C18 column and gradient elution (solvent A: phosphate buffer, pH 3.5 and solvent B: methanol) keeping a flow rate of 1.5 mL/min. Detection was done at dual wavelength (232 nm for domperidone and sodium benzoate, and 257 nm for sodium methylparaben and sodium propylparaben). Analysis time was < 17 min. The retention times for domperidone, sodium benzoate, sodium methylparaben and sodium propylparaben were found to be 10.0, 6.5, 8.0, and 13.5 min, The calibration curves for domperidone, sodium benzoate, sodium methylparaben and sodium propylparaben were found to be linear in the range of 250-750, 50-150, 50-150, and 5-15 μg/mL, respectively.

scholarly journals Potential Assessment of UGT2B17 Inhibition by Salicylic Acid in Human Supersomes In Vitro

Molecules ◽  
2021 ◽  
Vol 26 (15) ◽  
pp. 4410
Author(s):  
Hassan Salhab ◽  
Declan P. Naughton ◽  
James Barker
Keyword(s):  
Enzyme Activity ◽  
Salicylic Acid ◽  
Gradient Elution ◽  
Potential Effect ◽  
Reversed Phase ◽  
Hplc Method ◽  
Phase System ◽  
Testosterone Metabolism ◽  
Limit Values

Glucuronidation is a Phase 2 metabolic pathway responsible for the metabolism and excretion of testosterone to a conjugate testosterone glucuronide. Bioavailability and the rate of anabolic steroid testosterone metabolism can be affected upon UGT glucuronidation enzyme alteration. However, there is a lack of information about the in vitro potential assessment of UGT2B17 inhibition by salicylic acid. The purpose of this study is to investigate if UGT2B17 enzyme activity is inhibited by salicylic acid. A UGT2B17 assay was developed and validated by HPLC using a C18 reversed phase column (SUPELCO 25 cm × 4.6 mm, 5 μm) at 246 nm using a gradient elution mobile phase system: (A) phosphate buffer (0.01 M) at pH = 3.8, (B) HPLC grade acetonitrile and (C) HPLC grade methanol. The UGT2B17 metabolite (testosterone glucuronide) was quantified using human UGT2B17 supersomes by a validated HPLC method. The type of inhibition was determined by Lineweaver–Burk plots. These were constructed from the in vitro inhibition of salicylic acid at different concentration levels. The UGT2B17 assay showed good linearity (R2 > 0.99), acceptable recovery and accuracy (80–120%), good reproducibility and acceptable inter and intra-assay precision (<15%), low detection (6.42 and 2.76 μM) and quantitation limit values (19.46 and 8.38 μM) for testosterone and testosterone glucuronide respectively, according to ICH guidelines. Testosterone and testosterone glucuronide were found to be stable up to 72 h in normal laboratory conditions. Our investigational study showed that salicylic acid uncompetitively inhibited UGT2B17 enzyme activity. Thus, drugs that are substrates for the UGT2B17 enzyme have negligible potential effect of causing interaction with salicylic acid in humans.

scholarly journals Development and Validation of an HPLC Method for Simultaneous Quantification of Clopidogrel Bisulfate, Its Carboxylic Acid Metabolite, and Atorvastatin in Human Plasma: Application to a Pharmacokinetic Study

2015 ◽  
Vol 2015 ◽  
pp. 1-12 ◽  
Author(s):  
Octavian Croitoru ◽  
Adela-Maria Spiridon ◽  
Ionela Belu ◽  
Adina Turcu-Ştiolică ◽  
Johny Neamţu
Keyword(s):  
Carboxylic Acid ◽  
Internal Standard ◽  
Gradient Elution ◽  
Reversed Phase ◽  
Hplc Method ◽  
Acid Metabolite ◽  
Buffer Solution ◽  
Solution Ph ◽  
Limit Of Quantification ◽  
Simultaneous Quantification

A simple, sensitive, and specific reversed phase liquid chromatographic method was developed and validated for simultaneous quantification of clopidogrel, its carboxylic acid metabolite, and atorvastatin in human serum. Plasma samples were deproteinized with acetonitrile and ibuprofen was chosen as internal standard. Chromatographic separation was performed on an BDS HypersilC18column (250 × 4.6 mm; 5 μm) via gradient elution with mobile phase consisting of 10 mM phosphoric acid (sodium) buffer solution (pH = 2.6 adjusted with 85% orthophosphoric acid) : acetonitrile : methanol with flow rate of 1 mL·min−1. Detection was achieved with PDA detector at 220 nm. The method was validated in terms of linearity, sensitivity, precision, accuracy, limit of quantification, and stability tests. Calibration curves of the analytes were found to be linear in the range of 0.008–2 μg·mL−1for clopidogrel, 0.01–4 μg·mL−1for its carboxylic acid metabolite, and 0.005–2.5 μg·mL−1for atorvastatin. The results of accuracy (as recovery) with ibuprofen as internal standard were in the range of 96–98% for clopidogrel, 94–98% for its carboxylic acid metabolite, and 90–99% for atorvastatin, respectively.

scholarly journals Robust optimization of gradient RP HPLC method for simultaneous determination of ivabradine and its eleven related substances by AQbD approach

2021 ◽  
Author(s):  
Jovana Tomić ◽  
Nevena Djajić ◽  
Danica Agbaba ◽  
Biljana Otašević ◽  
Andjelija Malenović ◽  
...  
Keyword(s):  
Mobile Phase ◽  
Ph Value ◽  
Complex Mixture ◽  
Gradient Elution ◽  
Reversed Phase ◽  
Hplc Method ◽  
Elution Time ◽  
Optimal Separation ◽  
Rp Hplc ◽  
Final Amount

AbstractThis paper is aimed at developing a gradient elution reversed-phase high-performance liquid chromatography (RP-HPLC) method for the separation of a complex mixture composed of ivabradine and its eleven impurities, in a reasonable timeframe. In order to obtain a robust and reliable HPLC method for separation of this mixture, Analytical Quality by Design (AQbD) was applied. This approach demonstrated to be useful in development of a long lasting life cycle methods. Four chromatographic variables were defined as key method parameters (KMPs) and optimized towards the analytical target profile (ATP). Designated KMPs were initial and final amount of acetonitrile in the mobile phase, pH value of the aqueous phase and gradient time, while resolutions of critical peak pairs were denoted as critical method attributes (CMAs). Relationships between KMPs and CMAs were obtained with the aid of Design of Experiments (DoEs) methodology among which Box-Behnken design (BBD) was employed to gain valid mathematical models. Obtained mathematical equations were used to construct the Design Space (DS) and select reliable optimal separation conditions. They included 11% (v/v) and 34% (v/v) of initial and final amount of acetonitrile, respectively, as well as 45 min of gradient elution time and 20 mM ammonium acetate as aqueous mobile phase with pH set to 7.35. The possibility to separate the diastereoisomers of impurity X was also evaluated. It was demonstrated that this separation could not be achieved in gradient elution mode within the defined variable domains and in a reasonable time span. The developed method was validated according to ICH Q2 (R1) guideline and met all the required criteria.

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