scholarly journals Simultaneous HPTLC Determination of Rhein and Aloe-emodin in Senna Alata Leaves from Thailand and their Commercial Products

2017 ◽  
Vol 12 (3) ◽  
pp. 1934578X1701200
Author(s):  
Savita Chewchinda ◽  
Pongtip Sithisarn
Keyword(s):  
High Performance ◽  
Raw Materials ◽  
Commercial Products ◽  
Average Percentage ◽  
System Validation ◽  
Relative Standard ◽  
Aloe Emodin ◽  
Senna Alata ◽  
Hptlc Method

A high performance thin layer chromatographic (HPTLC) method was developed and validated for simultaneous determination of rhein and aloe-emodin, major anthraquinone constituents, in S. alata leaves. The separation was performed on a silica gel 60 F254 HPTLC plate using ethyl acetate: methanol: water (100:17:10, v/v/v) as the development system. Validation of the analytical method for rhein and aloe-emodin promoted acceptable parameters. Good linearity in the range of 40–480 ng/band was obtained while intra-day and inter-day precisions were shown to be precise with relative standard deviations of less than 5%. The average percentage recoveries of rhein and aloe-emodin were 98.8% and 98.9%, suggesting acceptable accuracy. The content of rhein and aloe-emodin in S. alata leaves collected from 5 different provinces in Thailand analyzed by the validated HPTLC method were in the ranges of 0.098 ± 0.017 −0.30 ± 0.02%, w/w, and 0.081 ± 0.0006 - 0.34 ± 0.0009 %, w/w, respectively. Five commercial products of S. alata tea available in the market were purchased and analyzed for rhein and aloe-emodin contents. The contents of rhein and aloe-emodin in the tea samples were in the ranges of 0.085 ± 0.004 - 0.23 ± 0.04%, w/w, and 0.096 ± 0.006 - 0.30 ± 0.01 %, w/w, respectively. The HPTLC method is rapid, reliable, sensitive and economical for routine analysis of rhein and aloe-emodin contents in S. alata leaf raw materials and its commercial products.

scholarly journals A Validated High-Performance Thin-Layer Chromatographic Method for the Simultaneous Determination of Zofenopril Calcium and Hydrochlorothiazide in the Presence of the Hydrochlorothiazide Impurities: Chlorothiazide and Salamide

2018 ◽  
Vol 101 (4) ◽  
pp. 1031-1041 ◽  
Author(s):  
Mamdouh R Rezk ◽  
Ahmed S Fayed ◽  
Hoda M Marzouk ◽  
Samah S Abbas
Keyword(s):  
Simultaneous Determination ◽  
High Performance ◽  
Degradation Products ◽  
Raw Materials ◽  
Drug Product ◽  
Hplc Method ◽  
Pharmaceutical Formulation ◽  
Significant Difference ◽  
Hptlc Method

Abstract The chromatographic analysis of either process-related impurities or degradation products is very important in the pharmaceutical industry. In this work, a simple, selective, and sensitive HPTLC method was developed and validated for the simultaneous determination of zofenopril calcium (ZOF) and hydrochlorothiazide (HCT) in the presence of the HCT impurities: A) chlorothiazide (CT) and B) salamide, in raw materials and in pharmaceutical formulation. The separation was carried out on HPTLC silica gel 60 F254 using ethyl acetate–glacial acetic acid–triethylamine (10 + 0.1 + 0.1, v/v/v) as a developing system. The separated bands were scanned densitometrically at 270 nm. Polynomial equations were used for the regression. Calibration curves were constructed for ZOF, HCT, CT, and salamide in the ranges of 0.5–10, 0.2–4, 0.05–1.4, and 0.05–1.0 μg/band, respectively. Different parameters affecting the suggested method, including developing systems of varying composition/ratios and different detection wavelengths, were studied to achieve the best resolution and precision with good sensitivity. System suitability parameters were also tested. The proposed method was validated as per the International Conference on Harmonization guidelines and was successfully applied for the quantification of the studied drugs in their pharmaceutical formulation, with no interference from excipients observed. The results obtained by the developed HPTLC method were compared statistically with those obtained by the reported HPLC method using Student’s t and F ratio tests, and no significant difference was obtained, indicating the ability of the proposed method to be used for routine analysis of drug product.

scholarly journals Single Laboratory Validation of a Method for Determination of Glucosamine in RawMaterials and Dietary Supplements Containing Glucosamine Sulfate and/or Glucosamine Hydrochloride by High-Performance Liquid Chromatography with FMOC-Su Derivatization

2004 ◽  
Vol 87 (5) ◽  
pp. 1083-1092 ◽  
Author(s):  
Joseph ZiQi Zhou ◽  
Ted Waszkuc ◽  
Felicia Mohammed
Keyword(s):  
High Performance Liquid Chromatography ◽  
Liquid Chromatography ◽  
Dietary Supplements ◽  
High Performance ◽  
Raw Materials ◽  
Glucosamine Sulfate ◽  
Glucosamine Hydrochloride ◽  
Relative Standard ◽  
Single Laboratory

Abstract Single laboratory validation of a method for determination of glucosamine in raw materials and dietary supplements containing glucosamine sulfate and/or glucosamine hydrochloride by with high-performance liquid chromatography FMOC-Su derivatization. Tests with 2 blank matrixes containing SAMe, vitamin C, citric acid, chondroitin sulfates, methylsulfonylmethane, lemon juice concentrate, and other potential interferents showed the method to be selective and specific. Eight calibration curves prepared over 7 working days indicated excellent reproducibility with the linear range at least over 2.0–150 μg/mL, and determination coefficients >0.9999. Average spike recovery from the blank matrix (n = 8 over 2 days) was 93.5, 99.4, and 100.4% at respective spike levels of 15, 100, and 150%, and from the sample matrix containing glucosamine (n = 3) was 99.9 and 102.8% at respective levels of 10 and 40%, with relative standard deviations <0.9%. The method was also applied to 12 various glucosamine finished products and raw materials. The stability tests confirmed that glucosamine–FMOC-Su derivative once formed is stable at room temperature for at least 5 days. Limit of quantitation was 1 μg/mL and limit of detection was 0.3 μg/mL. The method is ready to proceed for the collaborative study.

scholarly journals Quantitative Determination of Arbutin and Hydroquinone in Different Plant Materials by HPLC

2012 ◽  
Vol 40 (2) ◽  
pp. 109 ◽  
Author(s):  
Izabela RYCHLINSKA ◽  
Slawomira NOWAK
Keyword(s):  
High Performance ◽  
Raw Materials ◽  
Hplc Method ◽  
Fast Method ◽  
Optimum Conditions ◽  
Plant Materials ◽  
Ledum Palustre ◽  
Relative Standard ◽  
First Time

A simple, fast method of high-performance liquid chromatography for the determination and quantification of arbutin and hydroquinone in many different raw materials was developed and validated. The optimum conditions for the separation and detection of these two constituents were achieved on a LiChro-CARD 125-4 Superspher®100 RP-18 column with the water-methanol (gradient elution) mobile phase and recorded at 289 nm. The purities of peaks were verified by PDA analysis of impurities. The results of validation have shown that the HPLC method is stable and accurate for the simultaneous determination of arbutin and hydroquinone in extracts from various plants. The developed method gave a good sensitivity (LOD 1µg/ml for arbutin and 0.49 µg/ml for hydroquinone) with linearity R2 >0.9993 (for both). The relative standard deviation of the method was less than 2.53% for intra-day assays and 3.23% for inter-day assay, the accuracy of the recovery test ranged from 98.96% to 106.4%. This method was used in comparative qualitative analysis of arbutin and hydroquinone in 16 different raw materials from families Lamiaceae, Ericacaeae, Saxifragaceae, Rosaceae. The content of arbutin in B. ciliata, B. cordifolia and Ledum palustre was examined for the first time.

Method for the Determination of Lycopene in Supplements and Raw Material by Reversed-Phase Liquid Chromatography: Single-Laboratory Validation

2008 ◽  
Vol 91 (6) ◽  
pp. 1284-1297 ◽  
Author(s):  
André Müller ◽  
Bernd Pietsch ◽  
Nicole Faccin ◽  
Joseph Schierle ◽  
Edward H Waysek
Keyword(s):  
Dietary Supplements ◽  
High Performance ◽  
Raw Materials ◽  
Reversed Phase ◽  
Raw Material ◽  
Intermediate Precision ◽  
Relative Standard ◽  
Product Forms ◽  
Single Laboratory

Abstract A single-laboratory validation study was conducted for a liquid chromatographic (LC) method for the determination of total and all-trans-lycopene in a variety of dietary supplements and raw materials. Gelatin-based and other water-dispersible beadlets, or tablets, capsules, and softgels containing such product forms, were digested with protease. Alginate formulations and the respective applications were treated with an alkaline sodium EDTA acetate buffer to release lycopene from the matrix. Lycopene and other carotenoids were extracted from the resulting aqueous suspensions with dichloromethane and ethanol. Oily product forms were directly dissolved in dichloromethane and ethanol. The extracts were chromatographed on an isocratic high-performance LC system using a C16 alkylamide modified silica column that provided satisfactory resolution of all-trans-lycopene from its predominant cis-isomers and separated the lycopene isomers from other carotenoids such as - and -carotene, cryptoxanthin, lutein, and zeaxanthin. The within-day precision relative standard deviation (RSD) for the determination of total lycopene ranged from 0.9 to 5.7 over concentration ranges of 50200 g/kg for raw materials and 0.324 g/kg for dietary supplements. The intermediate precision RSD (total RSD) ranged from 0.8 to 8.9. Recoveries obtained for beadlet and tablet material for the different extraction variants ranged from 95.0 to 102.1 at levels of 0.0220 g/kg for tablets and from 95.0 to 101.1 at levels of 1200 g/kg for beadlet material.

A Validated Green HPTLC Method for Quantitative Determination of Dapoxetine Hydrochloride and Tadalafil in Bulk and Pharmaceutical Formulations

2020 ◽  
Vol 58 (4) ◽  
pp. 303-308 ◽  
Author(s):  
Ibrahim A Naguib ◽  
Maimana A Magdy ◽  
Basma H Anwar ◽  
Nessreen S Abdelhamid
Keyword(s):  
Quality Control ◽  
Mobile Phase ◽  
High Performance ◽  
Raw Materials ◽  
Pharmaceutical Formulations ◽  
Uv Detector ◽  
Ich Guidelines ◽  
Hptlc Method ◽  
Dapoxetine Hydrochloride

Abstract Dapoxetine hydrochloride (DAP) and Tadalafil (TAD) were separated and determined quantitatively using a validated green high-performance thin layer chromatographic (HPTLC) method in their binary mixtures either as raw materials or in pharmaceutical formulations. The concentration ranges were 0.1–1.6 and 0.2–2.5 μg/band for dapoxetine and tadalafil, respectively, with accuracies of 98.93% ± 0.62 and 99.26% ± 1.39, respectively. Silica gel HPTLC F254 plates were used to carry out the separation. The mobile phase used was a mixture of ethanol–ethyl acetate (1:9 by volume), which is environmentally green and harmless. Densitometric scanning with UV detector was used to detect the separated peaks at 222 nm. ICH guidelines were followed to validate the suggested method, and the results prove that they can be used for regular analysis in quality control laboratories with compatible results.

scholarly journals Determination of Glucosamine in Raw Materials and Dietary Supplements Containing Glucosamine Sulfate and/or Glucosamine Hydrochloride by High-Performance Liquid Chromatography with FMOC-Su Derivatization: Collaborative Study

2005 ◽  
Vol 88 (4) ◽  
pp. 1048-1058 ◽  
Author(s):  
Joseph Ziqi Zhou ◽  
Ted Waszkuc ◽  
Felicia Mohammed ◽  
M Blumhorst ◽  
R Buren ◽  
...  
Keyword(s):  
High Performance Liquid Chromatography ◽  
Liquid Chromatography ◽  
Dietary Supplements ◽  
High Performance ◽  
Raw Materials ◽  
Collaborative Study ◽  
Test Results ◽  
Commercial Products ◽  
Glucosamine Hydrochloride

Abstract A collaborative study was conducted for determination of glucosamine in raw materials and dietary supplements containing glucosamine sulfate and/or glucosamine hydrochloride by high-performance liquid chromatography (HPLC) with N-(9-fluorenyl-methoxycarbonyloxy) succinimide (FMOC-Su) derivatization. Thirteen blind materials, one pair of which were duplicates, were tested by 12 collaborating laboratories. The test samples consisted of various commercial products, including tablets, capsules, drink mix, and liquids as well as raw materials, blanks, and those for spike recovery analyses. The tests with blank products and products spiked with glucosamine showed good specificity of the method. The average recoveries at spike levels of 100 and 150% of the declared amount were 99.0% with a relative standard deviation (RSD) of 2.1%, and 101% with an RSD of 2.3%, respectively. The test results between laboratories on each commercial product were reproducible with RSD values of no more than 4.0%, and the results were repeatable in the same laboratory with an average RSD of 0.7%. HorRat values ranged from 0.5 to 1.7 on both tests of spike recovery and reproducibility between laboratories on commercial products. The average determination coefficient of the calibration curves from the laboratories was 0.9995 with an RSD of 0.03%. All of the 12 collaborating laboratories succeeded in the study and none of their reported test results were outliers, partly indicating the robustness of the method. It is recommended that the method be accepted by AOAC INTERNATIONAL as Official First Action.

scholarly journals Determination of Hydrastine and Berberine in Goldenseal Raw Materials, Extracts, and Dietary Supplements by High-Performance Liquid Chromatography with UV: Collaborative Study

2008 ◽  
Vol 91 (4) ◽  
pp. 694-701 ◽  
Author(s):  
Paula N Brown ◽  
Mark C Roman ◽  
C Chang ◽  
C Jin ◽  
R Kuriyedath ◽  
...  
Keyword(s):  
Dietary Supplements ◽  
High Performance ◽  
Raw Materials ◽  
Collaborative Study ◽  
High Performance Liquid Chromatographic ◽  
Hplc Method ◽  
Uv Detection ◽  
Acetonitrile Solution ◽  
Relative Standard

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.

scholarly journals Determination of Lycopene in Dietary Supplements and Raw Materials by High-Performance Liquid Chromatography: Collaborative Study

2010 ◽  
Vol 93 (2) ◽  
pp. 499-509 ◽  
Author(s):  
Edward H Waysek ◽  
Joseph Schierle ◽  
Andre Duesterloh ◽  
Jayant Deshpande ◽  
John Austad ◽  
...  
Keyword(s):  
Dietary Supplements ◽  
High Performance ◽  
Raw Materials ◽  
Collaborative Study ◽  
Negative Control ◽  
Study Results ◽  
Relative Standard ◽  
Lycopene Content ◽  
Standard Deviations

Abstract A collaborative study was conducted to evaluate the interlaboratory performance of an LC method for lycopene in dietary supplements and the raw materials commonly used in their manufacture. Twelve laboratories from six countries agreed to participate in the study. Results from 10 laboratories were received and are reported. Five dietary supplements, including both tablets and a softgel capsule with a lycopene content ranging from 25 g to 25 mg per unit, and three raw materials, including gelatin-based beadlets, vegetarian beadlets, and a suspension in oil ranging from 5 to 20 lycopene, were analyzed as blind duplicates. In addition to the commercial products, two positive controls and a negative control were included in the study. For the raw materials studied, the repeatability relative standard deviations (RSDr) ranged from 1.49 to 5.13 for total lycopene, and the reproducibility relative standard deviations (RSDR) ranged from 3.84 to 9.21 with HorRat values from 1.23 to 3.24. For finished products, the RSDr ranged from 1.31 to 4.62, RSDR from 4.28 to 10.5, and HorRat values from 0.79 to 2.07. Corresponding values for all-trans-lycopene were significantly higher. It is recommended that the method be considered for Official First Action for all-trans- and total lycopene in finished products and raw materials.

scholarly journals Determination of Coenzyme Q10 Content in Raw Materials and Dietary Supplements by High-Performance Liquid Chromatography-UV: Collaborative Study

2008 ◽  
Vol 91 (4) ◽  
pp. 702-708 ◽  
Author(s):  
Steven Lunetta ◽  
Mark Roman ◽  
A Chandrah ◽  
T Edamura ◽  
T Honda ◽  
...  
Keyword(s):  
Dietary Supplements ◽  
Coenzyme Q10 ◽  
High Performance ◽  
Raw Materials ◽  
Collaborative Study ◽  
Negative Control ◽  
Test Material ◽  
Relative Standard ◽  
Standard Deviations

Abstract An international collaborative study was conducted of a high-performance liquid chromatographic (HPLC)-UV method for the determination of coenzyme Q10 (CoQ10, ubidecarenone) in raw materials and dietary supplements. Ten collaborating laboratories determined the total CoQ10 content in 8 blind duplicate samples. Sample materials included CoQ10 raw material and 4 finished product dietary supplements representing softgels, hardshell gelatin capsules, and chewable wafers. In addition, collaborating laboratories received a negative control and negative control spiked with CoQ10 at low and high levels to determine recovery. Materials were extracted with an acetonitriletetrahydrofuranwater mixture. Ferric chloride was added to the test solutions to ensure all CoQ10 was in the oxidized form. The HPLC analyses were performed on a C18 column using UV detection at 275 nm. Repeatability relative standard deviations (RSDr) ranged from 0.94 to 5.05. Reproducibility relative standard deviations (RSDR) ranged from 3.08 to 17.1, with HorRat values ranging from 1.26 to 5.17. Recoveries ranged from 74.0 to 115. Based on these results, the method is recommended for Official First Action for determination of CoQ10 in raw materials and dietary supplement finished products containing CoQ10 at a concentration of >100 mg CoQ10/g test material.

Development of Validated Stability Indicating HPTLC Method for Assay of Ozagrel and its Pharmaceutical Formulations

2018 ◽  
pp. 36-48 ◽  
Author(s):  
Vishal N Kushare ◽  
Sachin S Kushare
Keyword(s):  
High Performance ◽  
Linear Regression Analysis ◽  
Pharmaceutical Formulations ◽  
Base Hydrolysis ◽  
Assay Method ◽  
Related Substance ◽  
Stability Indicating ◽  
Regular Production ◽  
Hptlc Method

The present paper describes stability indicating high-performance thin-layer chromatography (HPTLC) assay method for Ozagrel in bulk drugs. The method employed TLC aluminium plates precoated with silica gel 60F-254 as the stationary phase. The solvent system consisted of toluene: methanol: triethylamine (6.5: 4.0: 0.1 v/v/v). The system was found to give compact spot for Ozagrel (Rf value of 0.40 ± 0.010). Densitometric analysis of Ozagrel was carried out in the absorbance mode at 280 nm. The linear regression analysis data for the calibration plots showed good linear relationship with r2 = 0.999 with respect to peak area in the concentration range 30 - 120 ng/spot. The developed HPTLC method was validated with respect to accuracy, precision, recovery and robustness. Also to determine related substance and assay determination of Ozagrel that can be used to evaluate the quality of regular production samples. The developed method can also be conveniently used for the assay determination of Ozagrel in pharmaceutical formulations. The limits of detection and quantitation were 4.069 and 12.332 ng/spot, respectively by height. Ozagrel was subjected to acid and alkali hydrolysis, oxidation, photochemical and thermal degradation. The drug undergoes degradation under acidic, basic, oxidation and heat conditions. This indicates that the drug is susceptible to acid, base hydrolysis, oxidation and heat. Statistical analysis proves that the method is repeatable, selective and accurate for the estimation of said drug. The proposed developed HPTLC method can be applied for identification and quantitative determination of Ozagrel in bulk drug and tablet formulation.

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