scholarly journals Simultaneous determination of Rutin, Hesperidin and Quercetin contents in solid dietary supplements by high performance liquid chromatography

Author(s):  
Thanh Phuong Nguyen Thi ◽  
Hong Hanh Nguyen Thi ◽  
Thu Dam Thi ◽  
◽  
◽  
...  

Simultaneous determination of rutin, hesperidin and quercetin contents in several solid dietary supplement samples is possible by HPLC method. The analysis process usedthe Agilent Zorbax Eclipse XDB C18 column (250 x 4.6 mm; 5 µm), a mobile phase composed of acetonitrile - phosphoric acid solution 0.1% with gradient program. The detection was carried out on a DAD detector at 280 nm for hesperidin and at 254 nm for rutin and quercetin. The limit of quantitation of method was at a low level of concentration (0.021g/100g with rutin, 0.047g/100g with hesperidin and 0.0054g/100g with quercetin); the accuracy of the method was within 97.0 - 101.33%; the precision showed 1.11 - 1.92% of relative standard deviation which showed high repeatability of the method. The method was applied to 20 dietary supplements samples, the results indicated a high level for the selectivity and reliability of the method to be applied.

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.


2015 ◽  
Vol 3 ◽  
pp. 21-26
Author(s):  
Om Prakash Sharma ◽  
Nanthanit Pholphana ◽  
Nuchanart Rangkadilok ◽  
Preeda Parkpian ◽  
Jutamaad Satayavivad

The purpose of this study was to develop a simple and sensitive high performance liquid chromatography (HPLC) method for determination of glyphosate (GP) residues in soybean grains. From soybean matrix, glyphosate was extracted with a mixture of water and methanol (4:1, v/v) from soybean samples followed by protein precipitation with equal volume of methanol. No preconcentration and further clean up of the sample were required. Pre-column derivatization was carried out with excess amount of 9- fluorenylmethyl chloroformate (FMOC-Cl) in the presence of borate buffer. The gradient program developed in this method was successfully applied to a reverse phase HPLC system with a C18 column (ACE 5 μm 4.6 x 250 mm), and eluted with a mobile phase consisting of 50 mM phosphate buffer, pH 2.5, and acetonitrile at the flow rate of 0.8 ml/min and fluorescence detection. Parameters and conditions affecting extraction, derivatization reaction and chromatographic separation were systematically examined. Linearity of the method ranged from 0.005 - 1.0 μg/ml. The correlation coefficient (r2) of calibration curve for glyphosate in soybean sample was found to be 0.99929. The limit of detection (LOD) and limit of quantitation (LOQ) values were determined to be 0.125 mg/kg and 0.25 mg/kg, respectively. Average recovery was 95.2%. Repeatability and intermediate precision calculated on the basis of peak area were excellent and showed relative standard deviation ranged from 0.15 - 1.29% and 1.15 - 3.87%, respectively. The developed method has been successfully applied for determination of glyphosate residues in soybean grains obtained from Thailand and Nepal. Soybean samples (53) from two different lots were analyzed and glyphosate residues ranged from 0.23 mg/kg to 5.06 mg/kg. Almost 50% soybean samples contained nearly consistent residue levels in both lots but in remaining samples there was a significant variation of glyphosate levels between two lots. Relatively higher residues were detected in samples from Thailand (0.27-5.06 mg/kg) compared to Nepal (0.23-0.99 mg/kg). The results suggest that the proposed method can be used to determine glyphosate residues in foods derived from soybean and other crops such as corn, cotton, wheat, etc. where glyphosate is widely applied to these crops.


2021 ◽  
Vol 59 (5) ◽  
pp. 445-451
Author(s):  
Emad M Abd Elhalim ◽  
Mohamed A Amin ◽  
Mohamed A Ali

Abstract A rapid and accurate high-performance liquid chromatographic method was developed for the determination of both abamectin and closantel in the veterinary formulation. The chromatographic separation was conducted on an Agilent 1200 with a UV detector using Waters C18 (4.6 mm × 50 mm; 2.7 μm). The mobile phase consisted of acetonitrile:water (80:20 v/v) adjusts pH 3.0 using diluted phosphoric acid. The flow rate of 1.5 mL min−1 was used. An injection volume of 10 μL was used The calibration curve of abamectin B1b was linear with a correlation coefficient (r2) = 0.9996; over a concentration range of 2.0–8.0 μg/mL, abamectin B1a was linear with a correlation coefficient (r2) = 0.9997; over a concentration range of 8.0–32.0 μg/mL; with a retention time of 2.18 and 3.72 minutes for avermectin B1b and avermectin B1a, respectively. While the calibration curve of closantel was linear with a correlation coefficient (r2) = 0.99929; over a concentration range of 250.0–1,000.0 μg/mL for; with a retention time of 5.84 minutes. Correlation coefficient was r2 ≥ 0.999. The relative standard deviation was found to be ≤ 2. The proposed method was validated and successfully applied for the simultaneous determination of abamectin and closantel in the veterinary formulation.


2020 ◽  
Author(s):  
Sherin Farouk Hammad ◽  
Inas Abdallah ◽  
Alaa Bedair ◽  
Fotouh Mansour

Abstract Salting-out induced liquid-liquid microextraction method has been developed for plasma sample treatment before determination of alogliptin by high performance liquid chromatography with UV detection. Several parameters were optimized to achieve maximum enrichment, including type of extractant, volume of extractant, type of anion, type of cation, salt amount and pH. The optimum conditions were attained using 500 µL of acetonitrile, added to 1 mL of aqueous sample containing 250 mg of sodium chloride at pH 12. An RP-HPLC method was developed and validated according to the International Conference on Harmonization guidelines M10. The method was linear in the concentration range of 0.1 to 50 µg/mL (correlation coefficient= 0.997). The limit of detection was 19 ng/mL and limit of quantitation was 60 ng /mL. The method was accurate and precise with an average % recovery of 99.7% and a % relative standard deviation ranging between 1.5 and 2.5. These results showed that the salting-out induced liquid-liquid microextraction methods could be better than other sample preparation protocols in terms of sensitivity, easiness, solvent consumption and waste reduction.


2020 ◽  
Author(s):  
Sherin Farouk Hammad ◽  
Inas Abdallah ◽  
Alaa Bedair ◽  
Fotouh Mansour

Abstract Salting-out induced liquid-liquid microextraction method has been developed for plasma sample treatment before determination of alogliptin by high performance liquid chromatography with UV detection. Several parameters were optimized to achieve maximum enrichment, including type of extractant, volume of extractant, type of anion, type of cation, salt amount and pH. The optimum conditions were attained using 500 µL of acetonitrile, added to 1 mL of aqueous sample containing 250 mg of sodium chloride at pH 12. An RP-HPLC method was developed and validated according to the International Conference on Harmonization guidelines M10. The method was linear in the concentration range of 0.1 to 50 µg/mL (correlation coefficient= 0.997). The limit of detection was 0.019 µg/mL and limit of quantitation was 0.06 µg/mL. The method was accurate and precise with an average % recovery of 99.7% and a % relative standard deviation ranging between 1.5 and 2.5. These results showed that the salting-out induced liquid-liquid microextraction methods could be better than other sample preparation protocols in terms of sensitivity, easiness, solvent consumption and waste reduction.


2008 ◽  
Vol 91 (4) ◽  
pp. 694-701 ◽  
Author(s):  
Paula N Brown ◽  
Mark C Roman ◽  
C Chang ◽  
C Jin ◽  
R Kuriyedath ◽  
...  

Abstract A multilaboratory collaborative study was conducted on a high-performance liquid chromatographic (HPLC) method utilizing UV detection, previously validated using AOAC single-laboratory validation guidelines for determination of hydrastine and berberine in goldenseal (Hydrastis canadensis L.) raw materials, extracts, and dietary supplements at levels ranging from 0.4 to 6 (w/w). Nine collaborating laboratories determined the hydrastine and berberine content in 8 blind samples. Sample materials included powdered botanical raw materials, whole root material, and 4 finished product dietary supplements containing either goldenseal powdered root material or extract. The materials were extracted with an acidified water and acetonitrile solution. HPLC analyses of the extracts were performed on a C18 column using UV detection at 230 nm. Results for powdered root material and capsule products ranged from about 0.2 (w/w) for each alkaloid to about 4 (w/w) for each alkaloid. Liquid tincture results were approximately 40005000 g/mL for each alkaloid. Reproducibility relative standard deviations (RSDR) for hydrastine ranged from 2.68 to 6.65, with HorRat values ranging from 0.77 to 1.89. RSDR for berberine ranged from 5.66 to 7.68, with HorRat values ranging from 1.32 to 2.12. All finished products containing goldenseal extract yielded HorRat values <2.0. Based on these results, the method is recommended for Official First Action for determination of hydrastine and berberine in goldenseal raw materials and dietary supplement finished products containing powdered goldenseal and goldenseal extract.


BMC Chemistry ◽  
2021 ◽  
Vol 15 (1) ◽  
Author(s):  
Sherin F. Hammad ◽  
Inas A. Abdallah ◽  
Alaa Bedair ◽  
Fotouh R. Mansour

AbstractSalting-out induced liquid–liquid microextraction method has been developed for plasma sample treatment before determination of alogliptin by high performance liquid chromatography with UV detection. Several parameters were optimized to achieve maximum enrichment, including type of extractant, volume of extractant, type of anion, type of cation, salt amount and pH. The optimum conditions were attained using 500 µL of acetonitrile, added to 1 mL of aqueous sample containing 250 mg of sodium chloride at pH 12. An RP-HPLC method was developed and validated according to the International Conference on Harmonization guidelines M10. The method was linear in the concentration range of 0.1 to 50 µg/mL (correlation coefficient = 0.997). The limit of detection was 0.019 µg/mL and limit of quantitation was 0.06 µg/mL. The method was accurate and precise with an average % recovery of 99.7% and a % relative standard deviation ranging between 1.5 and 2.5. These results showed that the salting-out induced liquid–liquid microextraction methods could be better than other sample preparation protocols in terms of sensitivity, easiness, solvent consumption and waste reduction.


2020 ◽  
Author(s):  
Sherin Farouk Hammad ◽  
Inas Abdallah ◽  
Alaa Bedair ◽  
Fotouh Mansour

Abstract Salting-out induced liquid-liquid microextraction method has been developed for plasma sample treatment before determination of alogliptin by high performance liquid chromatography with UV detection. Several parameters were optimized to achieve maximum enrichment, including type of extractant, volume of extractant, type of anion, type of cation, salt amount and pH. The optimum conditions were attained using 500 µL of acetonitrile, added to 1 mL of aqueous sample containing 250 mg of sodium chloride at pH 12. An RP-HPLC method was developed and validated according to the International Conference on Harmonization guidelines M10. The method was linear in the concentration range of 0.1 to 50 µg /mL (correlation coefficient= 0.997). The limit of detection was 0.019 µg/mL and limit of quantitation was 0.06 µ g/mL. The method was accurate and precise with an average % recovery of 99.7% and a % relative standard deviation ranging between 1.5 and 2.5. These results showed that the salting-out induced liquid-liquid microextraction methods could be better than other sample preparation protocols in terms of sensitivity, easiness, solvent consumption and waste reduction.


2020 ◽  
Author(s):  
Sherin Farouk Hammad ◽  
Inas Abdallah ◽  
Alaa Bedair ◽  
Fotouh Mansour

Abstract Salting-out induced liquid-liquid microextraction method has been developed for plasma sample treatment before determination of alogliptin by high performance liquid chromatography with UV detection. Several parameters were optimized to achieve maximum enrichment including type of extractant, volume of extractant, type of anion, type of cation, salt amount and pH. The optimum conditions were achieved using 500 µL of acetonitrile, added to 1 mL of aqueous sample containing 250 mg of sodium chloride at pH 12. An RP-HPLC method was developed and validated according to the International Conference on Harmonization guidelines Q2 (R1). The method was linear in the concentration range of 0.1 to 50 µg/mL (correlation coefficient= 0.997). The limit of detection was 19 ng/mL and limit of quantitation was 60 ng /mL. The method was accurate and precise with a % recovery of 99.7% and a % relative standard deviation ranging between 1.5 and 2.5. These results showed that the salting-out induced liquid-liquid microextraction methods could be better than other sample preparation protocols in terms of sensitivity, easiness, solvent consumption and waste reduction.


2022 ◽  
Vol 20 (2) ◽  
pp. 383-387
Author(s):  
Yahia Z. Tabaza ◽  
Kamal M. Mansi ◽  
Hanan A. Azzam ◽  
Farah F. Al-Mamoori ◽  
Ali M. Al-Samydai ◽  
...  

Purpose: To develop a reversed phase high performance liquid chromatography (HPLC) method for the determination of dehydroepiandrosterone (DHEA) in dietary supplements. Methods: A reversed-phase high performance liquid chromatography (HPLC) method was developed for the determination of DHEA in dietary supplements. An isocratic system consisting of methanol and water (70:30 v/v) was run at a flow rate of 1 mL/min on a C18 HPLC column to achieve the separation. The method was validated with regard to linearity, intra-day and inter-day precision, and limits of both detection and quantification. Results: The method achieved a retention time of 10.8 min, a resolution of 4.12, a detection limit (LOD) of 50 ng/μL, a quantification limit (LOQ) of 166.7 ng/μL and a label claim of 108.6 % with a relative standard deviation (RSD) of 0.38 % over a range of 0.0625 – 0.50 mg/mL with a correlation coefficient of 0.9997. Conclusion: The method is simple, cost effective, time-saving and reliable for determining DHEA when compared to other reported methods in literature. Thus, it will be of benefit to manufacturers of this dietary supplement to adopt the method for quantitative laboratory analysis.


Sign in / Sign up

Export Citation Format

Share Document