scholarly journals Determination of Seven Flavonoids in Ixeridium gracile (DC.) Shih by High-Performance Liquid Chromatography

2009 ◽  
Vol 92 (3) ◽  
pp. 773-778 ◽  
Author(s):  
Juan Chen ◽  
Xue-Mei Ma ◽  
Yan-Ping Shi

Abstract A high-performance liquid chromatographic technique coupled with photodiode array detection was proposed for the simultaneous determination of 7 flavonoids, i.e., quercetin, kaempferol, 7-hydroxyflavanone, 7-methoxyflavanone, 2,4-dihydroxychalcone, 2,4-dihydroxydihydrochalcone, and 7,2-dihydroxy-3, 4-dimethoxyisoflavane, in extracts of the plant Ixeridium gracile. Optimum separation was obtained by using a reversed-phase C18 method. Because of the different UV characteristics of these components, 5 detection wavelengths were used for the quantitative analysis. All of the flavonoids showed good linearity (r > 0.9999). The limit of detection and limit of quantitation values for the analytes ranged from 0.06 to 0.46 g/mL and from 0.18 to 1.48 g/mL, respectively. The method was validated by evaluating repeatability, precision, stability, and accuracy. Five different extraction and purification procedures were investigated for preparation of the sample solution. The optimized method was applied to the determination of flavonoids in I. gracile and was found to be efficient.

2019 ◽  
Vol 31 (5) ◽  
pp. 1002-1008
Author(s):  
Somana Siva Prasad ◽  
G.V. Krishna Mohan ◽  
A. Naga Babu

A novel reversed-phase high performance liquid chromatographic (HPLC) technique for the determination of everolimus (Isomer-B) and its impurities in the tablet dosage form has been optimized using analytical quality by design (QbD) approach. All the compounds are monitored with the photodiode array (PDA) detector at 280 nm and the parameters namely; precision, accuracy, specificity, stability, linearity, limit of quantitation (LOQ) and limit of detection (LOD) are evaluated. The quantitation limits of IMP-A, IMP-B, IMP-C, IMP-D, IMP-E, Sirolimus and TGR are found to be 0.08, 0.08, 0.10, 0.10, 0.10, 0.08 and 0.08, respectively. Recovery studies from 0.9 mg/L to 9.0 mg/L are performed for all impurities and the values were obtained between 85-110 %. Injection volume and test concentrations have been optimized to achieve LOQ values under the reporting threshold. The whole technique is developed and validated as per International Council for Harmonization (ICH) guidelines. The proposed method is robust, sensitive, rapid and successful and helpful in the regions where regulatory agencies recommend HPLC analytical method.


2021 ◽  
Vol 9 (2) ◽  
Author(s):  
Darinka Brodnjak Vončina ◽  
Maša Islamčivic Razboršek ◽  
Marjana Simonič

The aim of this study was to develop a method for identification and quantification of phenolic acids in different wine samples. The simple reversed-phase HPLC-UV method for simultaneous determination of p-coumaric and ferulic acid was developed. The method was validated and working range, linearity, repeatability, accuracy, limit of quantitation LOQ and limit of detection LOD were determined. The linearity of the method was tested in concentration ranges 0.1-1 mg L-1 and 1-10 mg L-1. The correlation coefficients (r2) were greater than 0.996 and quality coefficients (QC) ≤ 5%. Detection limit for both compounds was 0.01 mg L-1. The method is precise (RSD


2017 ◽  
Vol 9 (2) ◽  
pp. 34
Author(s):  
N. Balaji ◽  
Sayeeda Sultana

Objective: An efficient, high performance liquid chromatographic method has been developed and validated for the quantification of related substances in pioglitazone hydrochloride drug substance.Methods: This method includes the determination of three related substances in pioglitazone hydrochloride. The mobile phase A is 0.1% w/v triethylamine in water with pH 2.5 adjusted by dilute phosphoric acid. The mobile phase B is premixed and degassed mixtures of acetonitrile and methanol. The flow rate was 1 ml/min. The elution used was gradient mode. The HPLC column used for the analysis was symmetry C18 with a length of 250 mm, the internal diameter of 4.6 mm and particle size of 5.0 microns.Results: The developed method was found to be linear with the range of 0.006-250% with a coefficient of correlation 0.99. The precision study revealed that the percentage relative standard deviation was within the acceptable limit. The limit of detection and limit of quantitation of the impurities was less than 0.002%and 0.006% with respect to pioglitazone hydrochloride test concentration of 2000 µg/ml respectively. This method has been validated as per ICH guidelines Q2 (R1).Conclusion: A reliable, economical HPLC method was magnificently established for quantitative analysis of related substances of pioglitazone hydrochloride drug substance.


2012 ◽  
Vol 1 (12) ◽  
pp. 410-413 ◽  
Author(s):  
Sukhbir Lal Khokra ◽  
Balram Choudhary ◽  
Heena Mehta

A rapid, simple and highly sensitive reversed phase high performance liquid chromatographic (RP-HPLC) method has been developed for the quantitative determination of Rabeprazole sodium and Aceclofenac in a combined dosage form. Rabeprazole sodium and Aceclofenac were chromatographed using C-18 column as stationary phase and methanol: acetonitrile: water (60 : 10 : 30 v/v/v) as the mobile phase at a flow rate of 1.0 ml/min at ambient temperature and detected at 280 nm. The retention time (RT) of Rabeprazole sodium and Aceclofenac were found to be 5.611 min and 2.102 minute, respectively. The linearities of Rabeprazole sodium and Aceclofenac were in the range of 1-10 µg/ml and 3-15 µg/ml, respectively. The limit of detection was found to be 0.091 µg/ml for Rabeprazole sodium and 0.043 µg/ml for Aceclofenac. The proposed method was applied for the determination of Rabeprazole sodium and Aceclofenac in a combined dosage form and result was found satisfactory.DOI: http://dx.doi.org/10.3329/icpj.v1i12.12450 International Current Pharmaceutical Journal 2012, 1(12): 410-413


2012 ◽  
Vol 10 (2) ◽  
pp. 67-70
Author(s):  
Abdullah Al Masud ◽  
Mohammad Saydur Rahman ◽  
Towfika Islam ◽  
Saki Sultana ◽  
Moynul Hasan ◽  
...  

A simple, reproducible and efficient reversed phase high performance liquid chromatographic (RPHPLC) method has been developed for the estimation of a recently approved anti allergic drug, amlexanox in oral paste dosage form. The separations were carried out on a Zorbax Eclipse XBD, C18 column (150 x 4.6 mm; 5?m) at a flow rate of 1.50 ml/min. by using mobile phase comprising of mixed buffer (pH adjusted to 6.50) and methanol (50:50 v/v). The injection volume was 10 ?l and the peaks were detected at 244 nm. The linear dynamic range found to be in the concentration range of 15-35 ?g/ml and coefficient of correlation was found to be 0.999. The %RSD value was below 2.0 for intra-day and inter-day precision which indicated that the method was highly precise. The LOD (Limit of detection) and LOQ (Limit of quantitation) were found to be 3.8 ng/ml and 12.5 ng/ml, respectively which revealed that the method was highly sensitive. The percentage recovery of amlexanox ranged from 99.31 to 99.75%, indicating the accuracy of the method and absence of interference from the excipients present in the formulation. The proposed method was simple, fast, accurate and reproducible and hence can be applied for routine quality control operations of amlexanox in oral paste dosage form. Key words: Amlexanox, Anti allergic, RP-HPLC, LOD, LOQ. DOI: http://dx.doi.org/10.3329/dujps.v10i2.11782 Dhaka Univ. J. Pharm. Sci. 10(2): 67-70, 2011 (December)


1977 ◽  
Vol 23 (11) ◽  
pp. 1984-1988 ◽  
Author(s):  
A M Krstulovic ◽  
P R Brown ◽  
D M Rosie ◽  
P B Champlin

Abstract Concentrations of total tryptophan were determined rapidly and sensitively in 50 microliter of serum by a reversed-phase partition version of high-performance liquid chromatography. For determination of total tryptophan, sample preparation requires only precipitation of the serum protein with trichloroacetic acid and removing excess trichloroacetic acid with a 1,1,2-trichlorotrifluoroethane(Freon)/tri-N-octylamine solution. Tryptophan in serum samples was detected by ultraviolet and fluorescence spectrometry. No interferences from the naturally occurring constituents of serum were observed. Elution time for tryptophan is 15 min, the limit of detection is 1 pmol.


1982 ◽  
Vol 28 (8) ◽  
pp. 1784-1787 ◽  
Author(s):  
J Lehmann ◽  
H L Martin

Abstract Tocopherols extracted from plasma with methanol or from platelets with chloroform/methanol were injected in methanol on a reversed-phase (C18) "high-performance" liquid-chromatographic column and eluted with water/methanol (2/98, by vol) at a flow rate of 1.4 mL/min. A "high-performance" spectrophotofluorometer was used for detection. Analytical recoveries ranged from 89 to 106%. The response was linear to at least 0.3 micrograms of either tocopherol (alpha- or gamma-) applied to the column, and the limit of detection was 0.1 ng. The method was used to measure tocopherols in plasma and platelets from human subjects, and some values are presented.


2013 ◽  
Vol 10 (3) ◽  
pp. 1014-1022
Author(s):  
Baghdad Science Journal

A simple, precise, rapid, and accurate reversed – phase high performance liquid chromatographic method has been developed for the determination of guaifenesin in pure from pharmaceutical formulations.andindustrial effluent. Chromatography was carried out on supelco L7 reversed- phase column (25cm × 4.6mm), 5 microns, using a mixture of methanol –acetonitrile-water: (80: 10 :10 v/v/v) as a mobile phase at a flow rate of 1.0 ml.min-1. Detection was performed at 254nm at ambient temperature. The retention time for guaifenesin was found 2.4 minutes. The calibration curve was linear (r= 0.9998) over a concentration range from 0.08 to 0.8mg/ml. Limit of detection (LOD) and limit of quantification ( LOQ) were found 6µg/ml and 18µg/ml respectively. The method was validated for its linearity, precision and accuracy .The proposed method was successfully applied for the determination of guaifenesin in syrups and industrial effluent samples.


2019 ◽  
Vol 34 (3) ◽  
pp. 172-180
Author(s):  
Galal Elmanfe ◽  
Suad K. Omar ◽  
Noreldin S.Y. Abdolla ◽  
Amna M. Hassan

The aim of the present study was to evaluate the levels of nicotine in twenty urine samples taken from ten smokers and ten non-smokers in Libya. Each volunteer was required to complete a questionnaire before providing the urine sample. The evaluation of the nicotine concentrations was carried out by means of a simple, rapid, cost effective but reliable, one-step extraction technique-reversed-phase high-performance liquid chromatography which was developed and validated for this purpose. The criteria and factors taken into consideration for this evaluation and validation include the linearity, precision, accuracy, limit of detection, and limit of quantitation. The urine samples from the smokers presented nicotine concentrations in the range of 0.037-1.979 µg/ml, with an average of 0.663 µg/ml. The range of the nicotine concentrations in non-smokers, on the other hand, was from 0.017-1.331 g/ml, where 0.273 µg/ml is the average value. Statistical analyses show that the nicotine concentrations were very significant in the smoker samples in contrast with the nonsmoker samples


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