Analysis of Piperine in Black Pepper by High Performance Liquid Chromatography

Piperine is the most important alkaloid present in the black pepper. A high performance liquid chromatography (HPLC) method proposed by International Organization for Standardization (ISO) was optimized and validated for quantitative determination of piperine in black pepper. The method was successfully validated for linearity, range, accuracy, precision, limit of detection, limit of quantitation, and measurement uncertainty. The validated method was used for the analysis of nine black pepper samples collected from the local supermarket of Kathmandu. The piperine content of the samples collected from various areas of Kathmandu, Nepal were found in the range of 2.33 % to 3.34 % with an average of 2.75 % and a standard deviation of 0.31%. This simple, precise, and accurate method can be used for routine analysis of piperine content in black pepper for quality control purposes.

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Development and Validation of Stability-Indicating Reverse Phase-High Performance Liquid Chromatography Method for Simultaneous Determination of Atenolol and Nifedipine in Bulk and Tablet Dosage Form

International Journal of Pharmaceutical Quality Assurance ◽

10.25258/ijpqa.11.2.4 ◽

2020 ◽

Vol 11 (02) ◽

pp. 219-223

Author(s):

Ansari Yaasir Ahmed ◽

Qazi Shoeb ◽

Umme Rumana ◽

Patel Afroza ◽

Pathan Vahid Tajkhan ◽

...

Keyword(s):

High Performance Liquid Chromatography ◽

Liquid Chromatography ◽

High Performance ◽

Dosage Form ◽

Limit Of Detection ◽

Hplc Method ◽

Forced Degradation ◽

Chromatography Method ◽

Stability Indicating ◽

Limit Of Quantitation

The new stability-indicating high performance liquid chromatography (HPLC) method has been developed and validated with different parameters for atenolol (ATE) and nifedipine (NIFE) in the combined dosage form. The chromatographic conditions were optimized using a mobile phase of MeOH:OPA (70:30) with a flow rate of 0.7 mL/min. Column (C18) of 4.6 × 250 mm dimension was used as a stationary phase; the particle size capacity of the column was 5 μm. The detection was carried out at 233 nm. The method was validated according to ICH guidelines for linearity, precision, repeatability, the limit of detection (LoD), and limit of quantitation (LoQ). The response was found to be linear in the concentration range of 20 to 100 mcg/mL for ATE and 1 to 5 mcg/mL for NIFE. The developed method shows the minimum quantity of drugs to be identified (LoD) and minimum drug to be quantified (LoQ). The LoD and LoQ were found to be 0.1415 and 0.4289, respectively, for ATE, and 0.1834 and 0.5558, respectively, for NIFE. The method was linear, simple, precise, and accurate and, therefore, suitable for routine analysis of drugs in tablet form. The forced degradation studies were also done through the exposure of analyte solution to four different stress conditions.

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Determination of Aflatoxin B1 in Feedstuffs without Clean-Up Step by High-Performance Liquid Chromatography

International Journal of Analytical Chemistry ◽

10.1155/2018/4650764 ◽

2018 ◽

Vol 2018 ◽

pp. 1-8 ◽

Cited By ~ 4

Author(s):

Sasiprapa Choochuay ◽

Jutamas Phakam ◽

Prakorn Jala ◽

Thanapoom Maneeboon ◽

Natthasit Tansakul

Keyword(s):

High Performance Liquid Chromatography ◽

Liquid Chromatography ◽

High Performance ◽

Limit Of Detection ◽

Precolumn Derivatization ◽

Broken Rice ◽

Relative Standard ◽

Limit Of Quantitation ◽

Aflatoxin B

A reliable and rapid method has been developed for the determination of aflatoxin B1 (AFB1) in four kinds of feedstuffs comprising broken rice, peanuts, corn, and fishmeal. A sample preparation was carried out based on the QuEChERS method with the exclusion of the clean-up step. In this study, AFB1 was extracted using acetonitrile/methanol (40/60 v/v), followed by partitioning with sodium chloride and magnesium sulfate. High-performance liquid chromatography with precolumn derivatization and fluorescence detection was performed. The coefficients of determination were greater than 0.9800. Throughout the developed method, the recovery of all feedstuffs achieved a range of 82.50-109.85% with relative standard deviation lower than 11% for all analytes at a concentration of 20-100 ng/g. The limit of detection (LOD) ranged from 0.2 to 1.2 ng/g and limit of quantitation (LOQ) ranged from 0.3 to 1.5 ng/g. The validated method was successfully applied to a total of 120 samples. The occurrence of AFB1 contamination was found at the following concentrations: in broken rice (0.44-2.33ng/g), peanut (3.97-106.26ng/g), corn (0.88-50.29 ng/g), and fishmeal (1.06-10.35 ng/g). These results indicate that the proposed method may be useful for regularly monitoring AFB1 contamination in feedstuffs.

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Identification, characterization, and determination of process-related impurities in Minodronic Acid bulk drug

Current Pharmaceutical Analysis ◽

10.2174/1573412917666210604160621 ◽

2021 ◽

Vol 17 ◽

Author(s):

Shi Anan ◽

Zou Qiaogen ◽

Gao Pan

Keyword(s):

High Performance Liquid Chromatography ◽

Liquid Chromatography ◽

High Performance ◽

Limit Of Detection ◽

Hplc Method ◽

Quantitative Detection ◽

Resonance Spectroscopy ◽

Related Impurities ◽

Minodronic Acid

Background: Minodronic acid (MA) is a third-generation nitrogen-containing heterocyclic bisphosphonate used to treat osteoporosis. In the process of starting materials research and preparation, the key intermediate impurities and degradation impurities have a great impact on the quality control of the drug. Objective: A sensitive, reliable high-performance liquid chromatography (HPLC) method was developed and validated for the quantitative determination of MA and its related impurities (a total of 6 compounds, including 2 new impurities). Methods: The separation was achieved on an InertSustain ODS-4 C18 (250 mm×4.6 mm, 5 μm) column using the mixture of 0.01 mol/L sodium pyrophosphate and 1 mmol tetrabutylammonium phosphate (the mobile phase pH was adjusted to 7.80 by phosphonic acid). Results: The quantitative analytical method was fully validated with respect to linearity (r>0.999), sensitivity (limit of detection<35 ng/mL), precision, accuracy (the recovery was between 98.7% and 104.2%), and robustness. Six process-related impurities in Minodronic Acid (MA) bulk drugs were determined by high-performance liquid chromatography (HPLC). Furthermore, except for two starting materials, other four impurities were identified and characterized as 2-(imidazo[1,2-a] pyridin-3-yl) ethyl acetate (Imp-C), 2-(imidazo [1,2-a] pyridin- 3-yl)acetic acid (Imp-D), 3-(2-hydroxy-2,2- diphosphonoethyl)-4H-imidazo [1,2-a] pyridine -4- oxide (Imp-E) and 2,5- Dihydroxy- 3,6-bis(imidazo[1,2-a] pyridine-3-yl methyl) -2,5-dioxo-1,4,2,5- dioxoDiphosphonium-3,6-diyl) bisphosphonic acid (Imp-F) using liquid chromatograph-mass spectrometer (LC-MS), MS/MS, Infrared Radiation and Nuclear Magnetic Resonance spectroscopy (1H-NMR and 13C-NMR). To the best of our knowledge, two of them (Imp-E and Imp-F) are new compounds and have not been reported previously. Conclusion: The HPLC method was developed and optimized, which could be applied for quantitative detection of the impurities, and further quality evaluation of MA.

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DETERMINATION OF INULIN FROM MULTIVITAMIN SYRUP PRODUCT BY HIGH PERFORMANCE LIQUID CHROMATOGRAPHY WITH RI DETECTOR

Indonesian Journal of Chemistry ◽

10.22146/ijc.21364 ◽

2012 ◽

Vol 12 (2) ◽

pp. 201-205 ◽

Cited By ~ 1

Author(s):

Yuni Retnaningtyas

Keyword(s):

High Performance Liquid Chromatography ◽

Liquid Chromatography ◽

High Performance ◽

Limit Of Detection ◽

Regression Function ◽

Hplc Method ◽

Limit Of Quantification ◽

Chromatography Method ◽

Label Claim

At present, inulin is often added to multivitamin syrup product. The determination of the component of preparation both qualitatively and quantitatively is important to ensure quality of the product. This research is aimed to develop a high performance liquid chromatography method to analyze inulin in multivitamin syrup preparation. Separation of inulin from the sample, was performed using Aminex column HPX-87H (300 x 7.8 mm) Ion Exclusion at a temperature of 80 °C with isocratic elution system using deionized water as mobile phase at a flow rate of 0.5 mL/min, and detected by using refractive index detector. This method validation showed a good linearity with correlation coefficient (r) of 0.999 while the coefficient of variation of the regression function (Vx0) was 2.00%. The limit of detection (LOD) and the limit of quantification (LOQ) of the method were respectively 0.12 mg/mL and 0.37 mg/mL. The mean absolute recovery of inulin from the simulation sample was 99.42% and the method precision was less than 2%. The proposed method has been applied to the determination of inulin in commercial multivitamin syrup and the recovery of label claim was 99.9 mg/100 mL. The proposed HPLC method is rapid, simple, and selective for routine analysis.

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Development of a Simple and Sensitive High-Performance Liquid Chromatography Method for Determination of Glucosamine in Pharmaceutical Formulations

Journal of AOAC International ◽

10.1093/jaoac/90.2.354 ◽

2007 ◽

Vol 90 (2) ◽

pp. 354-357 ◽

Cited By ~ 11

Author(s):

Mahboob Nemati ◽

Hadi Valizadeh ◽

Masood Ansarin ◽

Farank Ghaderi

Keyword(s):

High Performance Liquid Chromatography ◽

Liquid Chromatography ◽

High Performance ◽

Limit Of Detection ◽

Pharmaceutical Formulations ◽

Dosage Forms ◽

Detector Response ◽

Chromatography Method ◽

Limit Of Quantitation

Abstract A column high-performance liquid chromatography (HPLC) method was developed for the determination of glucosamine in dosage forms. Glucosamine was derivatized by addition of a solution containing orthophthaldialdehyde. The HPLC separation was achieved on a Spherimage 80 ODS2 column (250 4 mm id, 5 μm particle size) using an isocratic mobile phase containing phosphate buffermethanol (90 + 10, v/v, pH 6.50) and methanoltetrahydrofuran (97 + 3, v/v) in proportions of 85 + 15 at a flow rate of 1 mL/min, followed by fluorescence detection. The method was validated for specificity, linearity, accuracy, precision, limit of detection (LOD), and limit of quantitation (LOQ). The detector response for glucosamine HCl was linear over the concentration range of 0.120 μg/mL with a correlation coefficient of 0.9980. The accuracy was between 99.4 and 100.8%. The LOD and the LOQ were 0.009 and 0.027 μg/mL, respectively. The method was applied to determination of glucosamine in solid dosage forms.

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HPLC Determination of Formaldehyde in Flour Samples using 2,4,6-Trichlorophenyl Hydrazine as Derivatization Reagent

Asian Journal of Chemistry ◽

10.14233/ajchem.2021.23120 ◽

2021 ◽

Vol 33 (4) ◽

pp. 930-936

Author(s):

Khaldun M. Al Azzam ◽

Ahmad Makahleh ◽

Bahruddin Saad

Keyword(s):

High Performance Liquid Chromatography ◽

Liquid Chromatography ◽

Mobile Phase ◽

High Performance ◽

Limit Of Detection ◽

Hplc Method ◽

Limit Of Quantification ◽

Injection Volume ◽

Concentration Levels

A new simple and sensitive high-performance liquid chromatography (HPLC) method for the determination of formaldehyde in flour samples has been developed. Formaldehyde was quantified after derivatization with a readily available reagent, 2,4,6-trichlorophenyl hydrazine (TCPH) under basic conditions. The formaldehyde-TCPH derivative was eluted with chromatographic mobile phase of 70:30 (v/v) acetonitrile:water at a flow rate of 1.0 mL min–1; wavelength, 222 nm; injection volume, 50 μL, using a C18 ODS Hypersil column (250 mm × 4.5 mm, 5 μm). The calibration curve was linear over the range of 0.001-10 μg mL-1 with R2 = 0.999. Recoveries at three different concentration levels (0.1, 1.0 and 5 μg mL-1) ranged from 92.0-101.7% with RSD less than of 2.2%. The limit of detection (LOD) and limit of quantification (LOQ) were 0.3 and 1.0 ng mL-1, respectively. The developed method was used for the determination of formaldehyde in various flour-based samples.

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Developing a High-performance Liquid Chromatography Method for Simultaneous Determination of Loratadine and its Metabolite Desloratadine in Human Plasma

Current Drug Metabolism ◽

10.2174/1389200220666191125095648 ◽

2020 ◽

Vol 20 (13) ◽

pp. 1053-1059

Author(s):

Mahmoud M. Sebaiy ◽

Noha I. Ziedan

Keyword(s):

High Performance Liquid Chromatography ◽

Liquid Chromatography ◽

Human Plasma ◽

High Performance ◽

Allergic Diseases ◽

Reversed Phase ◽

Hplc Method ◽

H1 Receptor ◽

Chromatography Method

Background: Allergic diseases are considered as the major burden on public health with increased prevalence globally. Histamine H1-receptor antagonists are the foremost commonly used drugs in the treatment of allergic disorders. The target drug in this study, loratadine, belongs to this class of drugs and its biometabolite desloratadine which is also a non-sedating H1 receptor antagonist with anti-histaminic activity being 2.5 to 4 times greater than loratadine. This study aimed to develop and validate a novel isocratic Reversed-phase High-Performance Liquid Chromatography (RP-HPLC) method for rapid and simultaneous separation and determination of loratadine and its metabolite, desloratadine in human plasma. Methods: The drug extraction method from plasma was based on protein precipitation technique. The separation was carried out on a Thermo Scientific BDS Hypersil C18 column (5μm, 250 x 4.60 mm) in a mobile phase of MeOH: 0.025M KH2PO4 adjusted to pH 3.50 using orthophosphoric acid (85: 15, v/v) at an ambient temperature. The flow rate was maintained at 1 mL/min and maximum absorption was measured using the PDA detector at 248 nm. Results: The retention times of loratadine and desloratadine in plasma samples were recorded to be 4.10 and 5.08 minutes, respectively, indicating a short analysis time. Limits of detection were found to be 1.80 and 1.97 ng/mL for loratadine and desloratadine, respectively, showing a high degree of sensitivity of the method. The method was then validated according to FDA guidelines for the determination of the two analytes in human plasma. Conclusion: The results obtained indicate that the proposed method is rapid, sensitive in the nanogram range, accurate, selective, robust and reproducible compared to other reported methods.

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A Selective High-Performance Liquid Chromatography Method for the Determination of Reboxetine in Bulk Drug and Tablets

Journal of AOAC International ◽

10.1093/jaoac/89.6.1552 ◽

2006 ◽

Vol 89 (6) ◽

pp. 1552-1556

Author(s):

ArmaĞan Önal ◽

Olcay SaĞiri ◽

S Müge Çetin ◽

Sidika Toker

Keyword(s):

High Performance Liquid Chromatography ◽

Liquid Chromatography ◽

High Performance ◽

Depressive Disorders ◽

Degradation Products ◽

Severe Depression ◽

Hplc Method ◽

Chromatography Method ◽

Relative Standard

Abstract Reboxetine is used as a selective noradrenaline reuptake inhibitor for the treatment of major depressive disorders. It is effective in the treatment of severe depression and safer to use than traditional tricyclic antidepressants. In this study, a novel, simple, and rapid stability-indicating high-performance liquid chromatography (HPLC) method for reboxetine methansulfonate was successfully developed and validated for the assay of tablets. The method was used to quantify reboxetine in tablets; it employed a C18 column (150 4.6 mm id) with an isocratic mobile phase consisting of methanolphosphate buffer (pH 7, 0.02 M; 55 + 45, v/v) at a flow rate of 1.0 μmL/min. Reboxetine was detected by an ultraviolet detector at 277 nm. The retention time of reboxetine was about 4.5 min. The developed HPLC method was validated with respect to linearity, precision, sensitivity, accuracy, and selectivity. The method was linear over the concentration range 150 g/mL (r 0.9999). The limits of detection and the quantitation of reboxetine were 0.1 and 0.3 μg/mL, respectively. The relative standard deviation values for intraday and interday precision were 0.781.01 and 1.081.37%, respectively. Selectivity was validated by subjecting a stock solution of reboxetine to neutral, acid, and alkali hydrolysis, as well as oxidation, dry heat treatment, and photodegradation. The peaks of the degradation products did not interfere with the peak of reboxetine. The results indicated that the proposed method could be used in a stability assay. The proposed method was successfully applied to the determination of reboxetine in tablets. Excipients present in the tablets did not interfere with the analysis.

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Development of reverse phase-high performance liquid chromatography (RP-HPLC) method for determination of selected antihypertensive active flavonoids (rutin, myricetin, quercetin, and kaempferol) in medicinal plants found in Botswana

Physical Sciences Reviews ◽

10.1515/psr-2020-0209 ◽

2021 ◽

Vol 0 (0) ◽

Author(s):

Katso Binang ◽

David T. Takuwa

Keyword(s):

High Performance Liquid Chromatography ◽

Liquid Chromatography ◽

Medicinal Plants ◽

High Performance ◽

Zingiber Officinale ◽

Hplc Method ◽

Reverse Phase ◽

Rp Hplc ◽

Lippia Javanica

Abstract The aim of the study was to develop a rapid, efficient, and cheap chromatographic method for determining four selected antihypertensive active flavonoid compounds in medicinal plants in Botswana. The determination of rutin, quercetin, and kaempferol in selected medicinal plants was conducted in less than 6 min using the developed reverse phase-high performance liquid chromatography (RP-HPLC) method with a 2.7 µm Ascentis C18 express column (150 × 4.60 mm i.d) at 340, 360, and 368 nm detection wavelengths and mobile phase of methanol and 0.068% of formic acid solution in isocratic elution. Validation results showed good selectivity, linearity (r 2 > 0.99), high percentage recoveries (90.2–104.7%), and precision (% RSD < 2) for n = 3, confirming suitability of the method for determination of the investigated flavonoids in Zingiber officinale (ginger). Application of the developed RP-HPLC method was performed in selected medicinal plants (Lippia javanica ) (mosukujane), Myrothanmus flabellious (galalatshwene), and Elephantorrhiza elephantina (mositsana) used to manage hypertension by herbalists in Botswana. M. flabellious a very commonly used plant for managing hypertension was found to contain highest amounts of rutin and myricetin, whereas nothing was detected for E. elephantina.

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