scholarly journals Application of Hplc-Pda Method Using Two Different Extraction Procedures for the Determination of Alkylresorcinols in Cereals

2015 ◽  
Vol 69 (4) ◽  
pp. 182-189
Author(s):  
Natālija Gailāne ◽  
Ida Jākobsone ◽  
Vadims Bartkevičs ◽  
Ylle Tamm
Keyword(s):  
High Performance ◽  
Soxhlet Extraction ◽  
Extraction Methods ◽  
Photodiode Array Detection ◽  
Intermediate Precision ◽  
Chromatography Method ◽  
Extraction Procedures ◽  
Phenolic Lipids ◽  
Validation Parameters

Abstract Cereals, especially barley, are an important source of vitamins, minerals, dietary fibre and various phytochemicals, such as alkylresorcinols (ARs). Cereal ARs are a group of phenolic lipids located in the outer parts of grain, particularly in rye and wheat, but not found in refined flour or in refined products from cereals. This study focuses on the comparison of different extraction procedures applied for the determination of the content of ARs (C15:0 - C23:0) in grain of Latvian barley genotypes. The content of ARs in 1 rye and 16 barley samples grown with different amounts of fertilier was determined by High Performance Liquid Chromatography method with Photodiode Array detection (HPLC-PDA) developed by us. Two different extraction methods were compared: accelerated Soxhlet extraction and 24-hour extraction. Aside from validation of the extraction procedures, validation parameters for the HPLC-PDA based quantitation method were provided. The coefficients of variation for repeatability and intermediate precision were < 9% and < 3%, respectively. The content of ARs determined with the HPLC-PDA method in conjunction with accelerated Soxhlet extraction was up to 1.5 times higher than using 24-hour extraction. AR content varied from 2.11 ± 0.04 to 3.80 ± 0.10 mg·100 g-1 for 24-hour extraction and from 2.66 ± 0.06 to 5.70 ± 0.20 mg·100 g-1 for accelerated Soxhlet extraction, indicating the increased efficiency of this procedure in analysis of ARs.

scholarly journals The application of different methods for the determination of fat content in selected animal - origin products

2011 ◽  
Vol 27 (4) ◽  
pp. 1851-1852
Author(s):  
M. Surma-Zadora ◽  
K. Topolska ◽  
E. Cieślik ◽  
K. Sieja
Keyword(s):  
Soxhlet Extraction ◽  
Food Product ◽  
Extraction Methods ◽  
Fat Content ◽  
The Other ◽  
Animal Origin ◽  
Intermediate Precision ◽  
Food Composition Tables ◽  
Validation Parameters

The aim of the study was to assess the fat content in selected animal-origin products (ie. black pudding, luncheon, wiener, bacon) as well as certified reference material (MUVA RM700 Boiled Sausage) using two analytical methods. One of them was the fat extraction using a Soxhlet technique, and the other one - the extraction using carbon dioxide in supercritical state. Methods based on Soxhlet extraction have been and are at present used as reference. This conventional method is cheap and accurate, and this is why it has been the most used extraction technique worldwide for a number of decades. On the other hand some modern methods of fat determination are needed. Supercritical Fluid Extraction is quick, safe, and it eliminates any hazardous chemicals or solvents used in traditional extraction methods. For this purpose we used TFE 2000 fat analyzer (LECO Corporation). For the methods used the following validation parameters were determined: accuracy, precision, intermediate precision, correctness. The fat content in black pudding and luncheon meat ranged from 11.5 ? 4.5 g/100g (TFE) to 12.1 ? 0.0 g/100g (Soxhlet) and from 13.2 ? 0.5 g/100g (Soxhlet) to 13.8 ? 0.7 g/100g (TFE), respectively. For wiener samples we received values between 15.7 ? 0.4 g/100g (TFE) to 17.8 ? 0.1 g/100g (Soxhlet). The fat content in bacon samples ranged from 48.2 ? 2.5 g/100g (TFE) to 48.7 ? 0.7 g/100g (Soxhlet). The results received remain consistent with the values given in the Polish ?Food Composition Tables?. The application of the methods described above for the determination of fat content in animal - derived products is dependent ie.: on the purpose of analysis, the amount of fat in food product sample and the time for receiving the results.

scholarly journals A simple method for the quantification of diclofenac potassium in oral suspension by high-performance liquid chromatography with UV-detection

2013 ◽  
Vol 49 (3) ◽  
pp. 589-597 ◽  
Author(s):  
Alexandre Machado Rubim ◽  
Jaqueline Bandeira Rubenick ◽  
Luciane Varine Laporta ◽  
Clarice Madalena Bueno Rolim
Keyword(s):  
High Performance ◽  
Low Cost ◽  
Oral Suspension ◽  
Reverse Phase ◽  
Intermediate Precision ◽  
Simple Method ◽  
Ultraviolet Detection ◽  
Relative Standard ◽  
Validation Parameters

A rapid, simple and low cost method was developed to determine diclofenac potassium (DP) in oral suspension, using a reverse-phase column (C8, 150 mm x 4.6 mm, 5 µm), mobile phase containing methanol/buffer phosphate (70:30 v/v, pH 2.5), at a flow rate of 1.0 mL/min, isocratic method, and ultraviolet detection at 275 nm. A linear response (r = 1.0000) was observed in the range of 10.0-50.0 µg/mL. Validation parameters such as linearity, specificity, precision, accuracy and robustness were evaluated. The method presented precision (repeatability: relative standard deviation = 1.21% and intermediate precision: between-analyst = 0.85%). The specificity of the assay was evaluated by exposure of diclofenac potassium under conditions of stress such as hydrolysis, photolysis, oxidation and high temperature. The method presented accuracy values between 98.28% and 101.95%. The results demonstrate the validity of the proposed method that allows determination of diclofenac potassium in oral suspension and may be used as an alternative method for routine analysis of this product in quality control.

scholarly journals Validation of an HPLC method for the determination of amino acids in feed

2013 ◽  
Vol 78 (6) ◽  
pp. 839-850 ◽  
Author(s):  
Igor Jajic ◽  
Sasa Krstovic ◽  
Dragan Glamocic ◽  
Sandra Jaksic ◽  
Biljana Abramovic
Keyword(s):  
Amino Acids ◽  
High Performance ◽  
Limit Of Detection ◽  
High Specificity ◽  
Hplc Method ◽  
Array Detector ◽  
Limit Of Quantification ◽  
Intermediate Precision ◽  
Chromatography Method

The subject of this study is the validation of a high-performance liquid chromatography method for the analysis of amino acids in feed. The contents of amino acids were determined in maize, soybean, soybean meal, as well as in their mixtures enriched with different amounts of methionine, threonine and lysine. The method involves the acid hydrolysis of the sample (6 h at 150?C), automated derivatisation of amino acids with the aid of o-phthaldialdehyde and 9-fluorenylmethyl chloroformate reagents, separation on the ZORBAX Eclipse-AAA column, and detection using a diode-array detector. The method is characterized by high specificity (the difference between the retention times of the feed samples and standard mixtures are below 1.7 %), wide linear range (from 10 to 1000 nmol cm-3, r2 = 0.9999), high accuracy (recovery 93.3-109.4 %), and the precision of the results (RSD below 4.14 % in case of repeatability and below 4.57 % in the case of intermediate precision). The limit of detection and the limit of quantification are in the range 0.004-1.258 ?g cm-3 and 0.011-5.272 ?g cm-3, respectively. The results demonstrate that the procedure can be used as a method for the determination of the composition of primary amino acids of feed proteins.

scholarly journals ISOLASI DAN ANALISIS GENISTEIN DARI TEMPE BUSUK MENGGUNAKAN METODE KROMATOGRAFI KOLOM

2018 ◽  
Vol 5 (1) ◽  
pp. 88
Author(s):  
Hartati Soetjipto ◽  
Yohanes Martono ◽  
Zulfa Yuniarti
Keyword(s):  
Column Chromatography ◽  
Crude Extract ◽  
Mobile Phase ◽  
High Performance ◽  
Extraction Methods ◽  
Chromatography Method ◽  
Mobile Phases ◽  
Phase Combination ◽  
Layer Chromatography

Isolation and Analysis of Genistein of Overripe Tempe using Column Chromatography MethodABSTRACTGenistein is one of the aglycone isoflavone compounds in tempe that has various biochemical activities, including anticancer, antitumor, and antioxidants. Commonly used isoflavone extraction methods resulted in isoflavone crude extract. The aim of this study was to isolate the genistein of overripe tempe through determining the appropriate combination of mobile phases in genistein isolation and the determination of genistein content in both crude extract and isolate. The overripe tempe was first extracted, then genistein was isolated from the crude extract using column chromatography method. The determination of mobile phase combination was done by Thin Layer Chromatography while the genistein content was quantitatively determined by using High Performance Liquid Chromatography. The results showed that the appropriate combination of mobile phase for genistein isolation was chloroform : methanol (15 : 1, v/v). Genistein content in the crude extract and isolates were 4737.50 and 31.36 μg/g extract, respectively. The genistein purity in the isolates was 63.80%, while the purity in the isoflavone extract was 31.98%.Keywords: genistein, HPLC, isoflavone, overripe tempe, TLC ABSTRAKGenistein merupakan salah satu senyawa isoflavon aglikon dalam tempe yang memiliki bermacam-macam aktivitas biokimia, diantaranya antikanker, antitumor, dan antioksidan. Metode ekstraksi isoflavon yang umum diterapkan, menghasilkan ekstrak kasar isoflavon yang masih berupa campuran. Tujuan dari penelitian ini adalah untuk mengisolasi genistein dari tempe busuk melalui tahap penentuan kombinasi fase gerak yang tepat dalam isolasi genistein serta penentuan kandungan genistein baik dalam ekstrak kasar maupun isolat. Tempe busuk mula-mula diekstrak, selanjutnya genistein diisolasi dari ekstrak kasar menggunakan metode kromatografi kolom. Penentuan kombinasi fase gerak dilakukan secara Kromatografi Lapis Tipis, sedangkan kandungan genistein secara kuantitatif ditentukan dengan menggunakan Kromatografi Cair Kinerja Tinggi. Hasil penelitian menunjukkan bahwa kombinasi fase gerak yang tepat untuk isolasi genistein adalah kloroform : metanol (15 : 1, v/v). Kandungan genistein dalam ekstrak kasar dan isolat genistein berturut-turut sebesar 4737,50 dan 31,36 μg/g ekstrak. Kemurnian genistein dalam isolat adalah sebesar 63,80%, sedangkan kemurniannya dalam ekstrak isoflavon adalah sebesar 31,98%. Kata Kunci: genistein, HPLC, isoflavon, tempe busuk, KLT

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

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.

scholarly journals DETERMINATION OF 10-GINGEROL IN INDIAN GINGER BY VALIDATED HPTLC METHOD OF SAMPLES COLLECTED ACROSS SUBCONTINENT OF INDIA

2016 ◽  
Vol 8 (12) ◽  
pp. 190
Author(s):  
Kamran Ashraf ◽  
Syed Adnan Ali Shah ◽  
Mohd Mujeeb
Keyword(s):  
Thin Layer ◽  
Thin Layer Chromatography ◽  
High Performance ◽  
Limit Of Detection ◽  
Limit Of Quantification ◽  
Chromatography Method ◽  
Aluminum Plates ◽  
Layer Chromatography ◽  
Hptlc Method

<p><strong>Objective: </strong>A simple, sensitive, precise, and accurate stability indicating HPTLC (high-performance thin-layer chromatography) method for analysis of 10-gingerol in ginger has been developed and validated as perICH guidelines.</p><p><strong>Methods: </strong>The separation was achieved on TLC (thin layer chromatography) aluminum plates pre-coated with silica gel 60F<sub>254</sub> using n-hexane: ethyl acetate 55:45 (%, v/v) as a mobile phase. Densitometric analysis was performed at 569 nm.</p><p><strong>Results: </strong>This system was found to have a compact spot of 10-gingerol at <em>R</em><sub>F</sub> value of 0.57±0.03. For the proposed procedure, linearity (<em>r</em><sup>2</sup> = 0.998±0.02), limit of detection (18ng/spot), limit of quantification (42 ng/spot), recovery (ranging from 98.35%–100.68%), were found to be satisfactory.</p><p><strong>Conclusion: </strong>Statistical analysis reveals that the content of 10-gingerol in different geographical region varied significantly. The highest and lowest concentration of 10-gingerol in ginger was found to be present in a sample of Patna, Lucknow and Surat respectively which inferred that the variety of ginger found in Patna, Lucknow are much superior to other regions of India.</p>

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