Analytical method for the determination of curcumin entrapped in polymeric micellar powder using HPLC

2021 ◽  
Vol 32 (4) ◽  
pp. 867-873
Author(s):  
Helmy Yusuf ◽  
Nina Wijiani ◽  
Rizka Arifa Rahmawati ◽  
Riesta Primaharinastiti ◽  
M. Agus Syamsur Rijal ◽  
...  

Abstract Objectives Curcumin belongs to the family of curcuminoids, natural polyphenolic compounds that possesses neuroprotective properties, anti inflammatory and anticancer. Its entrapment in the developed casein-based micellar powder (CMP) and poloxamer-based micellar powder (PMP) was to enhance the solubility and improve the bioavailability. Henceforth, the present study aimed to acquire an efficient analytical method for the curcumin analysis in polymeric micellar formulations. Methods A fast and specific HPLC method was developed for analyzing curcumin in two different micellar matrices using casein and poloxamer. The HPLC was equipped with a C18 column (250 × 4 mm, 5 µm) and diode array detector. A designated isocratic elution of curcumin was employed using mobile phase with a composition of water (1%, v/v acetic acid) and acetonitrile in a ratio of 50:50 v/v. The employed flow rate was 1.0 mL/min and the analyte was examined at 421 nm. Results An effective analysis in HPLC was successfully achieved by the predetermined HPLC condition. A good resolution of peaks at the employed flow rate was achieved. The linearity was excellent in two different range of concentrations, 2–20 and 10–50 μg/mL. The selectivity, accuracy and precision fulfilled the acceptable requirements. Conclusions The developed method was practically effective to qualitatively identified curcumin. In addition, the assay also effectively quantified the amount of curcumin in the polymeric entrapping matrices which demonstrates that it has great potential to be used in natural compound analysis.


2016 ◽  
Vol 11 (11) ◽  
pp. 1934578X1601101 ◽  
Author(s):  
Derya Cicek Polat ◽  
Maksut Coskun

The genus Epimedium is rich in terms of flavonoids, of which icariin, epimedin A, epimedin B and epimedin C are known especially to be biologically active. Therefore, it is important to quantify these compounds. In this study, a HPLC method coupled with DAD detection was developed and validated for the determination of icariin, epimedin A, epimedin B and epimedin C in Epimedium species growing in Turkey. The chromatographic separation was performed using a gradient system with a mobile phase of 0.1% formic acid (A) and acetonitrile (B) applied at a flow rate of 1 mL/min using a diode array detector. The highest values were, respectively, icariin 0.65%, epimedin A 0.13%, epimedin B 0.11%, epimedin C 0.06%. The highest values were obtained from the materials collected in Uzungol (Trabzon-Turkey).



2013 ◽  
Vol 96 (3) ◽  
pp. 670-675 ◽  
Author(s):  
Balwinder Singh ◽  
Kousik Mandal ◽  
Sanjay K Sahoo ◽  
Urvashi Bhardwaj ◽  
Raminderjit Singh Battu

Abstract An easy and simple analytical method was standardized and validated for the estimation of residues of spirotetramat and its metabolite spirotetramat cis enol in various substrates: okra fruits, brinjal leaves and fruits, green chili, red chili, and soil. The samples were extracted with acetonitrile, diluted with brine solution, partitioned into dichloromethane, dried over anhydrous sodium sulfate, and cleaned up by treatment with activated charcoal powder. Final clear extracts were concentrated under vacuum and reconstituted with HPLC grade acetonitrile. Residues were estimated using HPLC with a photodiode array detector and a C18 column, and confirmed by HPTLC. Acetonitrile was used as the mobile phase at 0.4 mL/min. Both spirotetramat and spirotetramat cis enol presented distinct peak at retention times of 8.518 and 7.598 min, respectively. Consistent recoveries ranging from 82 to 97% for spirotetramat and spirotetramat cis enol were observed when samples were spiked at 1.00 to 0.03 mg/kg levels. The LOQ of the method was found to be 0.03 mg/kg. The analytical method was validated in terms of parameters, including selectivity, linearity, precision, and accuracy.



2009 ◽  
Vol 92 (4) ◽  
pp. 1089-1094
Author(s):  
Tai-Li Tsou ◽  
Chiu-Wey Lee ◽  
Hsian-Jenn Wang ◽  
Ya-Chung Cheng ◽  
Yu-Tien Liu ◽  
...  

Abstract A new HPLC method has been developed and validated for the simultaneous determination of ticarcillin (TIC) and clavulanic acid (CA) in pharmaceutical formulations. The HPLC separation was achieved on a -cyclodextrin column (Cyclobond I, 250 4.6 mm, 5 mm) with methanol16 mM pH 6.0 ammonium acetate buffer (50 + 50, v/v) mobile phase at a flow rate of 0.8 mL/min. Detection was at 220 nm. Validation of the method was performed by evaluating specificity, robustness, accuracy, and precision. The calibration curves were linear in the range of 1100 g/mL for CA and 2200 g/mL for TIC. The LOQs based on the standard regression lines were 0.42 and 1.42 g/mL for CA and TIC, respectively, and the LOD were 0.14 and 0.47 g/mL, respectively. Total recoveries of synthetic mixtures (CA:TIC = 1:10, 1:15, and 1:30) were 99.25100.99 for CA and 99.54100.82 for TIC. Compared with the U.S. Pharmacopeia method, the proposed method has the advantage of a relatively low flow rate and short analysis time. The proposed method was successfully applied for the simultaneous determination of these two drugs in sterilized H2O and 5 dextrose injection solutions.



2010 ◽  
Vol 93 (6) ◽  
pp. 1778-1787 ◽  
Author(s):  
Bharathi Avula ◽  
Yan-Hong Wang ◽  
Zulfiqar Ali ◽  
Ikhlas A Khan

Abstract An HPLC method was developed for the simultaneous determination of nine compounds of Nigella sativa L. The separation was achieved within 23 min by using C18 column material, a wateracetonitrile mobile phase, both containing 0.1 acetic acid gradient system and a temperature of 35C. The method was validated for linearity, repeatability, LOD, and LOQ. The LOD and LOQ of nine compounds were in the range of 0.0910 and 0.325 g/mL, respectively. The wavelength used for quantification with the diode array detector was 205 and 260 nm. LC/MS coupled with electrospray ionization interface method is described for the identification of compounds in N. sativa L. samples. This method involved the use of [MH]<sup/> and [MNa]<sup/> ions in the positive ion mode with extracted ion chromatogram.



INDIAN DRUGS ◽  
2012 ◽  
Vol 49 (07) ◽  
pp. 54-57
Author(s):  
P. Sathyanarayana ◽  
◽  
M Vijayalakshmi ◽  
B. N. V Ravi Kumar

A RP-HPLC method was developed and validated for the determination of ramosetron hydrochloride in pharmaceutical formulation as per ICH and FDA guidelines. The method was carried out on a Phenomenex RP-C18 column using a mixture of methanol and water (95:5) in an isocratic mode. The flow rate is 0.8 mL/min and the detection was done at 302 nm. The linearity range was observed in the range of 1-6 mcg/mL. The accuracy of the method was found to be 99.0 to 99.5% and %RSD was found to be less than 2% indicating high degree of accuracy and precision for the proposed HPLC method. Limit of detection and limit of quantification of the method were found to be 0.028 and 0.0851 mcg/mL respectively.



2014 ◽  
Vol 9 (8) ◽  
pp. 1934578X1400900
Author(s):  
Gulen Irem Kaya ◽  
Derya Cicek Polat ◽  
Buket Sarikaya ◽  
Mustafa Ali Onur ◽  
Nehir Unver Somer

Lycorine and galanthamine have various biological activities. A reliable HPLC method coupled with DAD detection was developed and validated for the determination of galanthamine and lycorine in Galanthus trojanus and G. cilicicus. A simple method for the extraction of the alkaloids in low-mass plant samples was employed utilizing columns pre-packed with diatomaceous earth (Extrelut®). This method was applied to the aerial parts and bulbs of G. trojanus and G. cilicicus (Amaryllidaceae) collected during the flowering season. The chromatographic separation was performed using an isocratic system with a mobile phase of trifluoroacetic acid-water-acetonitrile (0.01:92.5:7.5) applied at a flow rate of 1 mL min−1 and using a diode array detector. Validation procedures showed that the method was specific, accurate and precise. The highest amount of lycorine (0.012%) was detected in the bulbs of G. trojanus collected from Çan (Çanakkale), whereas the aerial parts of this species collected from Bayramiç (Çanakkale) was not found to contain this alkaloid. In G. cilicicus samples, lycorine was only determined in the bulbs, giving yields of 0.004%; galanthamine yields were between 0.015-0.016%, but none of the G. trojanus samples contained this latter alkaloid.



2013 ◽  
Vol 19 (No. 6) ◽  
pp. 201-205 ◽  
Author(s):  
R. Amarowicz ◽  
S. Weidner

Phenolic compounds were extracted from rye caryopses with 80% (v/v) methanol. Phenolic acids were determined as free compounds and those liberated from soluble esters and glycosides. The analyses were performed using a Waters HPLC system equipped with a diode array detector (DAD). The following free phenolic acids were found: p-coumaric, ferulic and sinapic; the phenolic acids liberated from soluble esters were as follows: vanillic, caffeic, p-coumaric, ferulic and sinapic; and those liberated from soluble glycosides were the following: vanillic, p-coumaric, ferulic and sinapic. In rye caryopses, phenolic acids were chiefly in the form of soluble esters. A diode array detector was especially useful for the determination of vanillic acid: the UV spectrum of this compound showed a maximum at 260 nm whereas UV spectra of other phenolic acids were characterised by maxima at longer wavelengths.



Author(s):  
Şule Dinç-Zor ◽  
Özlem Aksu Dönmez

Abstract Background The advantages of simultaneous analyses are a decrease in analysis time and a more economical use of solvents and reagents. It is desirable that HPLC analyses possess both short term and good resolution. Objective The aim of the current study is to develop an HPLC method for the simultaneous determination of ibuprofen, sodium benzoate, methyl paraben and propyl paraben as preservatives, and sunset yellow as a colorant, in syrup formulation. Method To optimize chromatographic separation conditions, multi-response optimization using the Derringer’s desirability function was employed for the development of a rapid and efficient HPLC method. The ranges of independent variables used for the optimization process were 50–60% (v/v) for acetonitrile, 5.0–7.0 for pH, and 1.0–2.0 mL/min for flow rate of the mobile phase. The effects of these variables on the output responses, such as critical resolution between sunset yellow and sodium benzoate and retention time of the last peak indicating analysis time of the method, were evaluated by statistical experimental design. Results Optimum conditions fixed for the simultaneous analyses were acetonitrile:phosphate buffer (60:40, v/v), pH 5.0, and a flow rate of 1.8 mL/min. The eluate was monitored using a photo diode detector set at 220 nm. Total chromatographic analysis time was approximately 3 min. Conclusions The developed method validated as per International Conference on Harmonization guidelines was successfully applied for the determination of five compounds in their pharmaceutical formulation. Highlights This efficient method has isocratic elution system and can be used for routine analyses of these compounds in similar pharmaceutical products.



Author(s):  
SYED IBRAHIM BAJE ◽  
B. JYOTHI ◽  
N. MADHAVI

Objective: The objective of the present study was to develop and validate a novel reverse phase high performance liquid chromatographic (RP-HPLC) method, for simultaneous determination of ritonavir (RIT), ombitasvir (OMB) and paritaprevir (PAR) in bulk mixtures, and in tablets. Methods: Determination of the drugs ritonavir (RIT), ombitasvir (OMB), and paritaprevir (PAR), was carried out applying Hypersil BDS C18 column (250 mm X 4.6 mm i.e., 5 µm particle size), with photodiode array detector at λmax of 254 nm. The mobile phase applied for the current study composed of two solvents, i.e. A (0.01N % w/v potassium di-hydrogen orthophosphate buffer, pH 3.0 adjusted with dilute orthophosphoric acid) and B (acetonitrile). The mobile phase was pumped at a flow rate of 1.0 ml/min in the isocratic mode. The validation study with respect to specificity, linearity, precision, accuracy, and robustness, limit of detection (LOD) and limit of quantification (LOQ) was carried out employing the ICH guidelines. Results: Ritonavir, ombitasvir, and paritaprevir showed linearity of response between 12.5-75 μg/ml for ritonavir, 3.125-18.75 µg/ml for ombitasvir and 18.75–112.5 µg/ml for paritaprevir, with a correlation coefficient (R2) 0.999, 0.999,0.999 for RIT, OMB, and PAR respectively. The % recovery obtained was 99.82±0.14 % RIT, OMB 100.03±0.96 % and for 99.96±0.26 % PAR. The LOD and LOQ values for RIT, OMB, PAR were obtained to be 0.02, 0.019and0.02, µg/ml and 0.07, 0.06 and 0.07 µg/ml, respectively. The method also exhibits good robustness for different chromatographic conditions like wavelength, flow rate, mobile phase, and injection volume. Conclusion: The method was successfully employed, for the quantification of RIT, OMB, and PAR, in the quality control of in-house developed tablets, and can be applied for the industrial use.



Author(s):  
Ajay Bedadurge ◽  
Kadare Mahesh ◽  
Vinod Matole ◽  
Parikshit Shirure ◽  
Sainath Suryawanshi ◽  
...  

The analytical method was developed and validated for determination of acyclovir in ointment by High performance liquid chromatography. The separation was carried out on Luna C18 column (250 × 4.6mm × 5µ). The mobile phase consists of water: acetonitrile in the ratio 88:12 at flow rate 0.8ml/min with diode array detector wavelength at 254nm.The column temperature was adjusted at 30ºC±40ºC with injection volume 20µl.The retention time of acyclovir was 4.747min. The linearity of the calibration curve was linear over the concentration range 80-120µg/ml (r2=0.9996). The validation was carried out as per ICH guidelines. The development method was easy, rapid, linear, precise, accurate and consistent.



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