scholarly journals Simultaneous Determination of Fish Steroidal Hormones using RP-HPLC with UV Detection by Multi-step Gradient Elution Technique

Author(s):  
Ningthoukhongjam Soranganba ◽  
I.J. Singh
2010 ◽  
Vol 48 (7) ◽  
pp. 589-594 ◽  
Author(s):  
M. S. Arayne ◽  
N. Sultana ◽  
F. A. Siddiqui ◽  
A. Z. Mirza ◽  
F. Qureshi ◽  
...  

2019 ◽  
Vol 102 (1) ◽  
pp. 69-74 ◽  
Author(s):  
Jianye Yan ◽  
Yuanqing Wang ◽  
Hongnian Wu ◽  
Zhicheng Sun ◽  
Shihan Tan ◽  
...  

Abstract Background: Polygonum Cuspidatum Sieb. et Zucc. (named Huzhang in China) is a traditional and popular Chinese medicinal herb used in removing jaundice, clearing heat-toxin, improving blood circulation, expelling stasis, dispelling wind and dampness, repelling phlegm, and suppressing cough. It is widely used in drug and functional food fields and distributed throughout the world, including in China, Japan, and North America. Objective: To control the quality of Polygonum Cuspidatum, an effective, reliable, and simple method for simultaneous determination of two stilbenes (polydatin, resveratrol) and four anthraquinones (emodin, physcion, rhein, and anthraglycoside B) was developed and validated for the first time in this study by reversed-phase HPLC (RP-HPLC). Methods: Separation was carried out on Agilent C18 column (250 × 4.6 mm I.D., 5 μm) with acetonitrile and 0.10% aqueous phosphoric acid as mobile phase and gradient elution at a flow rate of 0.8 mL/min. Detection was conducted with mobile wavelength at 30°C. Results: Good validation of the method including linearity, precision, repeatability, and recovery was performed. The contents of the studied analytes are significantly different, and resveratrol and rhein in particular existed in greater fluctuation among the samples. Conclusion: A simple, reliable, and sensitive method has been successfully established and applied to the analysis for simultaneous determination of the target compounds in 11 batches of samples. Highlights: Separation and quantitative analysis of two stilbenes and four anthraquinones from P. cuspidatum were developed by RP-HPLC. This method is convenient, sensitive, and accurate and can provide a reliable basis for further applications of P. cuspidatum in drug or food fields.


2020 ◽  
Vol 66 (1) ◽  
pp. 85-90
Author(s):  
Zhaklina Poposka Svirkova ◽  
Zorica Arsova-Sarafinovska ◽  
Aleksandra Grozdanova

Due to the low absorptivity of bile acids, the aim of this study was to develop and validate a simple and sensitive HPLC/UV method for quantification of ursodeoxycholic acid (UDCA) in pharmaceutical formulations. Effective separation was achieved on C18 end–capped column, with gradient elution of a mobile phase composed of 0.001 M phosphate buffer (pH 2.8±0.5) – acetonitrile mix, at flow rate 1.5 mL min-1, UV detection at 200 nm and injection volumes were 50 µL. The proposed HPLC method was fully validated according to the ICH guidelines and it was found to be simple, accurate, precise and robust. Key words: ursodeoxycholic acid, HPLC/UV, pharmaceutical formulations, validation


2014 ◽  
Vol 97 (3) ◽  
pp. 791-797 ◽  
Author(s):  
Hiral Soni ◽  
Charmy Kothari ◽  
Deepak Khatri ◽  
Priti Mehta

Abstract Validated RP-HPLC, HPTLC, and UV spectrophotometric methods have been developed for the simultaneous determination of atorvastatin calcium (ATV) and olmesartan medoxomil (OLM) in a pharmaceutical formulation. The RP-HPLC separation was achieved on a Kromasil C18 column (250 × 4.6 mm, 5 μm particle size) using 0.01 M potassium dihydrogen o-phosphate (pH 4 adjusted with o-phosphoric acid)–acetonitrile (50 + 50, v/v) as the mobile phase at a flow rate of 1.5 mL/min. Quantification was achieved by UV detection at 276 nm. The HPTLC separation was achieved on precoated silica gel 60F254 plates using chloroform–methanol–acetonitrile (4 + 2 + 4, v/v/v) mobile phase. Quantification was achieved with UV detection at 276 nm. The UV-Vis spectrophotometric method was based on the simultaneous equation method that involves measurement of absorbance at two wavelengths, i. e., 255 nm (λmax of OLM) and 246.2 nm (λmax of ATV) in methanol. All three methods were validated as per International Conference on Harmonization guidelines. The proposed methods were simple, precise, accurate, and applicable for the simultaneous determination of ATV and OLM in a marketed formulation. The results obtained by applying the proposed methods were statistically analyzed and were found satisfactory.


2012 ◽  
Vol 95 (2) ◽  
pp. 411-418 ◽  
Author(s):  
Tom Phillips ◽  
Adrian Burns ◽  
J Adams ◽  
O Bennett ◽  
M Curry ◽  
...  

Abstract Fourteen collaborating laboratories assayed o-phenylphenol (OPP), p-t-amylphenol (PTAP), and o-benzyl-p-chlorophenol (OBPCP) in formulated products, both ready-to-use and concentrates, by RP-HPLC. The actives in the samples ranged from 0.03 to 11% OPP, 0.06 to 4% PTAP, and 0.07 to 10% OBPCP either in free forms or as salts. Seven blind duplicates were analyzed. The samples were diluted/extracted with acidified methanol, filtered, and analyzed by LC on a C18 column using gradient elution and UV detection at 285 nm. The concentration of the active ingredients was calculated from a standard curve. Each laboratory weighed each test sample twice within a single analytical run. The data were analyzed using all 14 laboratory results, with appropriate statistical tests to detect outliers. The repeatability RSDs ranged from 0.98 to 3.40% for the free phenols, and 1.26 to 2.51% for the salts. The reproducibility RSDs ranged from 5.31 to 7.80% for the free phenols, and 5.50 to 8.67% for the salts. The HorRat ranged from 0.86 to 2.17 for the free phenols, and 1.54 to 2.72 for the salts.


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