scholarly journals Determination of protodioscin in tribulus terrestris by reversed-phase high-performance liquid chromatography

2021 ◽  
Vol 284 ◽  
pp. 03002
Author(s):  
Mikhail Sergeev ◽  
Georgiy Zaitsev ◽  
Dmitry Yermolin

In this study, high performance liquid chromatography (HPLC) was used to analyze the protodioscin content in Tribulus terrestris samples. They were separated by C18 chromatography column, gradient with 0.1 % phosphoric acid solution and acetonitrile was used as the mobile phase with the flow rate of 0.5 mL/min, the column temperature was 45 °C, and the detection wavelength was 203 nm. The results showed that the protodioscin content has a good linear correlation (r>0.999) within the range of 50 mg/L to 1500 mg/L. In samples of raw material from Crimea it was found: 0.546 % ± 0.013 protodioscin and in analyzed material from Western Siberia it was 0.338% ± 0.008 for n=3. Raw materials of Tribulus terrestris growing in Crimea are more promising than similar raw materials from the West Siberian region due to the higher content of protodioscin for the production of biologically active products containing steroid saponins.

2012 ◽  
Vol 9 (3) ◽  
pp. 1599-1604 ◽  
Author(s):  
Danijela A. Kostić ◽  
Snezana S. Mitić ◽  
Danijela Č. Nasković ◽  
Aleksandra R. Zarubica ◽  
Milan N. Mitic

A high-performance liquid chromatography (HPLC) system was used in the reversed phase mode for the determination of benzalkonium chloride (BKC) in nosal drops. A Chromolit RP-18e, 100 x 4.6, (UM6077/035) column was used at 40 °C. The mobile phase, optimized through an experimental design, was a 70:30 (v/v) mixture of 0.057M Na-heksansulphonate potassium, dihydrogen orthophosphate buffer (pH 2.9) and acetonitrile, pumped at a flow rate of 1.75 mL/min at maintaining column temperature at 40 °C. Maximum UV detection was achieved at 215 nm. The method was validated in terms of selectivity, linearity, repeatability, precision and accuracy. The method was successfully applied for the determination of BKC in a pharmaceutical formulation of nasal drop solution without any interference from common excipients and drug substance. All the validation parameters were within the acceptance range, concordant to ICH guidelines.


Author(s):  
Shaik Shakirbasha ◽  
Sravanthi P

  Objective: To develop and validate a simple, selective, precise, and accurate method for the estimation of dapagliflozin using reversed-phase high-performance liquid chromatography (RP-HPLC) technique in bulk and tablet formulation.Methods: The proposed method utilizes chromatographic conditions hypersil BDS (250 mm × 4.6 mm, 5 μ), mobile phase was buffer:acetonitrile (60:40) ratio, flow rate was maintained 1 ml/minute, column temperature was set at 30°C, detection wave length was 245 nm, and diluent was mobile phase.Results: By injecting 5 times of the standard solution system suitability parameters were studied, and results were found well under the acceptance criteria. The linearity study was performed by taking 25-150% levels, and the R2 value was found to be 0.999, precision was found to be 0.5 for repeatability and 0.31 for intermediate precision. The % recovery was found to be 99.89%. Limit of detection and limit of quantitation were found to be 0.60 μg/ml and 1.81 μg/ml, respectively. The % purity was found to be 99.71%. Degradation study on dapagliflozin was performed and concluded that the purity threshold was more than purity angle and within the acceptable range.Conclusion: The developed RP-HPLC method for dapagliflozin was found to be simple, precise, accurate, reproducible, and cost effective. Statistical analysis of the developed method conforms that the proposed method is an appropriate and it can be useful for the routine analysis. This method gives the basic idea to the researcher who is working in area such as product development and finish product testing.


2007 ◽  
Vol 90 (5) ◽  
pp. 1227-1236 ◽  
Author(s):  
Debra Orozco ◽  
Jules Skamarack ◽  
Kelly Reins ◽  
Barry Titlow ◽  
Steve Lunetta ◽  
...  

Abstract A method based on high-performance liquid chromatography with ultraviolet detection has been developed to quantify ubidecarenone [coenzyme Q10 (CoQ10)] in raw materials and dietary supplements. Single-laboratory validation has been performed on the method to determine repeatability, accuracy, selectivity, limits of detection and quantification (LOQ), ruggedness, and linearity for CoQ10. As CoQ10 can exist as the biologically active reduced form, the application of an oxidizing agent, ferric chloride, drives the equilibrium mechanics to the fully oxidized state and allows for exact quantification of total CoQ10 in the sample. This method was found to be fit and linear for the testing of materials containing CoQ10 in the range of 501000 mg/g. Repeatability precision for CoQ10 was between 2.15 and 5.00 relative standard deviation. Observed recovery of CoQ10 was found to be between 93.8 and 100.9. LOQ was found to be 9 g/mL. Further, limited studies showed that some adulterants and degraded material could be satisfactorily separated from CoQ10 and identified.


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