scholarly journals Quantitative determination of curcumin, demethoxycurcumin and bisdemethoxycurcumin from dietary supplements using HPLC-UV

2019 ◽  
Vol 2 (3) ◽  
pp. 10-17
Author(s):  
Giang Nguyen Huong ◽  
Nhan Do Ngoc ◽  
Son Pham Van ◽  
Duy Nguyen Bui ◽  
Lu Ngo Thi ◽  
...  
Keyword(s):  
Dietary Supplements ◽  
High Performance ◽  
Reliable Method ◽  
Ho Chi Minh City ◽  
Uv Detector ◽  
Limits Of Detection ◽  
Average Recovery ◽  
Real Samples ◽  
Relative Standard

A simple, sensitive and reliable method was developed and applied to determine curcumin, demethoxycurcumin (DMC) and bisdemethoxycurcumin (BDMC) (curcuminoid) in dietary supplements by High-Performance Liquid Chromatography using UV detector (HPLC-UV). The method was validated for linearity, repeatability, reproducibility, limits of detection and limits of quantification. The limits of detection and limits of quantification of curcuminoids were found to be 10 mg/kg and 40 mg/kg, respectively. The calibration curve showed good linearity for the three compounds (R2 > 0,999). The average recovery rates of curcuminoid at three spiked levels ranged from 90.3% to 106.7% and the relative standard deviations were less than 2.0%. The method has also been successfully applied to analyze curcuminoid in the real samples collected in Ho Chi Minh City.

ICH/FDA Guidelines-Compliant Validated Stability-Indicating HPLC-UV Method for the Determination of Axitinib in Bulk and Dosage Forms

2020 ◽  
Vol 16 (8) ◽  
pp. 1106-1112
Author(s):  
Ibrahim A. Darwish ◽  
Nasr Y. Khalil ◽  
Mohammad AlZeer
Keyword(s):  
High Performance ◽  
Kinase Inhibitor ◽  
Degradation Products ◽  
Internal Standard ◽  
Dosage Forms ◽  
Uv Detector ◽  
Stability Indicating ◽  
Therapeutic Benefits ◽  
Relative Standard

Background: Axitinib (AXT) is a member of the new generation of the kinase inhibitor indicated for the treatment of advanced renal cell carcinoma. Its therapeutic benefits depend on assuring the good-quality of its dosage forms in terms of content and stability of the pharmaceutically active ingredient. Objective: This study was devoted to the development of a simple, sensitive and accurate stabilityindicating high-performance liquid chromatographic method with ultraviolet detection (HPLC-UV) for the determination of AXT in its bulk and dosage forms. Methods: Waters HPLC system was used. The chromatographic separation of AXT, internal standard (olaparib), and degradation products were performed on the Nucleosil CN column (250 × 4.6 mm, 5 μm). The mobile phase consisted of water:acetonitrile:methanol (40:40:20, v/v/v) with a flow rate of 1 ml/min, and the UV detector was set at 225 nm. AXT was subjected to different accelerated stress conditions and the degradation products, when any, were completely resolved from the intact AXT. Results: The method was linear (r = 0.9998) in the concentration range of 5-50 μg/ml. The limits of detection and quantitation were 0.85 and 2.57 μg/ml, respectively. The accuracy of the method, measured as recovery, was in the range of 98.0-103.6% with relative standard deviations in the range of 0.06-3.43%. The results of stability testing revealed that AXT was mostly stable in neutral and oxidative conditions; however, it was unstable in alkaline and acidic conditions. The kinetics of degradation were studied, and the kinetic rate constants were determined. The proposed method was successfully applied for the determination of AXT in bulk drug and dosage forms. Conclusions: A stability-indicating HPLC-UV method was developed and validated for assessing AXT stability in its bulk and dosage forms. The method met the regulatory requirements of the International Conference on Harmonization (ICH) and the Food and Drug Administration (FDA). The results demonstrated that the method would have great value when applied in quality control and stability studies for AXT.

High Performance Liquid Chromatographic Determination of Primidone in Tablets

1982 ◽  
Vol 65 (5) ◽  
pp. 1063-1065
Author(s):  
Stanley E Roberts
Keyword(s):  
Mobile Phase ◽  
High Performance ◽  
Chromatographic Determination ◽  
High Performance Liquid Chromatographic ◽  
Hplc Method ◽  
Average Recovery ◽  
Relative Standard ◽  
Liquid Chromatographic Determination ◽  
Liquid Chromatographic

Abstract A high performance liquid chromatographic (HPLC) method is described for the quantitative determination of primidone in tablets. A ground tablet sample is diluted directly in the mobile phase, at a concentration of about 1 mg/mL of primidone, mixed and deaerated, and filtered. The resulting solution is then quantitated by HPLC. The average spike recoveries for the 50 mg and 250 mg tablets were 101.2% and 99.0%, respectively. The average recovery for an authentic mixture formulated at the 250 mg level was 100.1% with a relative standard deviation of 0.45%.

High-Performance Liquid Chromatography Quantitative Determination of Oxyresveratrol and Morin Contained in Maclura cochinchinensis Extract and Gel Formulation

2021 ◽  
Vol 901 ◽  
pp. 79-85
Author(s):  
Arpa Petchsomrit ◽  
Boonyadist Vongsak
Keyword(s):  
High Performance Liquid Chromatography ◽  
Liquid Chromatography ◽  
High Performance ◽  
Anticancer Activities ◽  
Limits Of Detection ◽  
Percent Recovery ◽  
Relative Standard ◽  
Traditional Drug ◽  
Detection And Quantification

Maclura cochinchinensis (Lour.) Corner., of the Moraceae family, is a medical shrub commonly found in Thailand, and for which a wide variety of pharmacological activities have been reported, including antiviral, anti-inflammatory, antioxidant, and anticancer activities. The main bioactive compounds, oxyresveratrol and morin, are known to be found in M. cochinchinensis heartwood. In this study, we quantitatively analyzed the levels of these two active substances in M. cochinchinensis extracted with various solvents, including in various cosmetic formulations and herbs sourced from various parts of Thailand. High-performance liquid chromatography (HPLC) was performed on a C18 column with an isocratic elution using 1.5% formic acid and acetonitrile at a flow rate of 1 ml/min, and detected at 352 nm. This method was validated for accuracy, precision, linearity, limits of detection, and quantification. The average percent recovery for oxyresveratrol and morin in the extracts was 100.01 ± 0.62% and 99.31 ± 2.56%, and in gel formulation was 99.65 ± 3.54% and 118.41 ± 4.70%, respectively. The relative standard deviation of intra- and inter-day precision was less than 2.0% and 2.8%, respectively. Limits of detection and quantification were 0.06 and 0.2 μg/ml, respectively. The amounts of oxyresveratrol and morin extracted from different solvents, such as acetone, 80% ethanol, 50% ethanol, methanol, and distilled water were in the range of 37.75–68.16 and 54.63–144.83 mg/g, respectively, while five samples of M. cochinchinensis heartwood collected from different regions of traditional drug stores contained in the range of 26.85–60.37 and 110.26–157.44 mg/g, respectively. Additionally, the percentage label amounts of oxyresveratrol and morin were analyzed in gel preparations, and found at 82.88% and 120.99%, respectively. This technique is convenient, simple, and reliable to effectively analyze the content of these active compounds in extracts and cosmetic products.

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.

Simultaneous Determination of Abamectin and Closantel in Veterinary Formulation by Validated HPLC Method

2021 ◽  
Vol 59 (5) ◽  
pp. 445-451
Author(s):  
Emad M Abd Elhalim ◽  
Mohamed A Amin ◽  
Mohamed A Ali
Keyword(s):  
Simultaneous Determination ◽  
Correlation Coefficient ◽  
Calibration Curve ◽  
Retention Time ◽  
High Performance ◽  
High Performance Liquid Chromatographic ◽  
Hplc Method ◽  
Uv Detector ◽  
Relative Standard

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.

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.

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

2020 ◽  
Vol 3 (1) ◽  
pp. 38-45
Author(s):  
Thanh Phuong Nguyen Thi ◽  
Hong Hanh Nguyen Thi ◽  
Thu Dam Thi ◽  
◽  
◽  
...  
Keyword(s):  
Dietary Supplements ◽  
Simultaneous Determination ◽  
High Performance ◽  
Hplc Method ◽  
Phosphoric Acid Solution ◽  
Analysis Process ◽  
Relative Standard ◽  
Limit Of Quantitation ◽  
High Level

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.

scholarly journals Analysis of fipronil and metabolites of fipronil in eggs by LC-MS/MS

2019 ◽  
Vol 2 (2) ◽  
pp. 29-36
Author(s):  
Giang Nguyen Huong ◽  
Nhan Do Ngoc ◽  
Son Pham Van ◽  
◽  
◽  
...  
Keyword(s):  
Liquid Chromatography ◽  
Calibration Curve ◽  
Reliable Method ◽  
Tandem Mass ◽  
Average Recovery ◽  
Real Samples ◽  
Good Linearity ◽  
Chicken Egg ◽  
Relative Standard ◽  
Liquid Chromatography Tandem Mass

A simple, sensitive and reliable method was developed and applied to determine fipronil and its metabolites in chicken egg by means of liquid chromatography-tandem mass spectrometry (LC-MS/MS). Chicken egg samples were extracted with water and acetonitrile, added with DisQuE salt, shaken and then centrifuged. The extracts were purified by Oasis cartridge prior to analysis by LC-MS/MS. The calibration curve showed good linearity within the concentrations from 0.5 to 10.0 µg/kg (R2 > 0.99). The average recovery rates of fipronil and its metabolites at three spiked levels of 2.0; 5.0 and 10.0 µg/kg ranged from 93.24 % to 107.89 % and the relative standard deviations were less than 9.2 %. The LOQ of this method was of 0.6 µg/kg and LOD was of 0.2 µg/kg. The method has also been successfully applied to analyze fipronil and its metabolites in the real samples.  

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.

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