Identification of coexisting pentose, hexose, and disaccharides with preliminary separation through hydrophilic interaction on silica HPTLC plate using aqueous sodium deoxycholate-acetonitrile mobile phase system

2011 ◽  
Vol 24 (6) ◽  
pp. 491-496 ◽  
Author(s):  
Ali Mohammad ◽  
Sameen Laeeq
Keyword(s):  
Mobile Phase ◽  
Sodium Deoxycholate ◽  
Phase System ◽  
Hydrophilic Interaction ◽  
Hptlc Plate ◽  
Aqueous Sodium ◽  
Preliminary Separation

scholarly journals Method validation for simultaneous quantification of some Human Milk Oligosaccharides (HMOs) in dietary supplements by liquid chromatography tandem mass spectrometry (LC-MS/MS)

2021 ◽  
Vol 4 (1) ◽  
pp. 24-26
Author(s):  
Hong Ngoc Nguyen Thi ◽  
Thanh Hoa Mac Thi ◽  
Son Tran Hung ◽  
Dung Ngo Manh ◽  
Khanh Cao Cong ◽  
...  
Keyword(s):  
Human Milk ◽  
Dietary Supplements ◽  
Mobile Phase ◽  
Food Samples ◽  
Phase System ◽  
Time Analysis ◽  
Simultaneous Quantification ◽  
Chromatography Tandem Mass Spectrometry ◽  
Validation Parameters ◽  
Liquid Chromatography Tandem Mass

The method of simultaneous quantification some of Human Milk Oligosaccharide in dietary supplements by LC-MS/MS is an accurate and effective method to quickly determine the content of 2'-Fucosyllactose (2 '-FL), Lacto-N-neotetraose (LNnT), Lacto-N-tetraose (LNT), 3'-Siallylactose (3'-SL) and 6'-Siallylactose (6'-SL) in both dietary supplements powder and liquid. The method has been developed and validated follow the AOAC International guidelines. The mobile phase system consists of 2 channels: channel A (0.1% formic acid) and channel B (acetonitril) connected to the HILIC column (3.5 μm, 2.1mm × 150 mm) and the MS detector. The time analysis is 10 minutes, this method can identify all 5 substances belonging to the group HMOs. The detection limit and quantitative limit for all 5’-FL, LNnT, LNT, 3’-SL, 6’-SL were 4 mg/kg and 10 mg/kg, respectively. The linear range of the method ranges from 0.4 µg/mL to 40 µg/mL. Other validation parameters include the accuracy (R% 98.8 -103%); The precision (RSD% 1.69 - 5.54%) can meet the requirement of AOAC. The method was applied in practice to analyze 25 supplementary food samples on the market gives the results of analyzing total HMOs in powdered samples about 0.1 – 0.3 g/100g and for liquid samples about 0.01 – 0.03 g/100mL.

scholarly journals ISOLATION, CHARACTERIZATION AND VALIDATION OF HPLC METHOD FOR QUANTIFICATION OF BIS-[10-(2-METHYL-4H-3-THIA-4,9-DIAZABENZO[F]AZULENE)]-1,4-PIPERAZINE IN AN ANTI-PSYCHOTIC DRUG SUBSTANCE, OLANZAPINE

2018 ◽  
Vol 10 (4) ◽  
pp. 22
Author(s):  
Suresh Babu Bodempudi ◽  
Ravi Chandra Babu Rupakula ◽  
Konda S. Reddy ◽  
Mahesh Reddy Ghanta
Keyword(s):  
Mobile Phase ◽  
Sodium Hydroxide Solution ◽  
Linear Regression Analysis ◽  
Sodium Dodecyl ◽  
Hplc Method ◽  
Drug Substance ◽  
Phase System ◽  
Column Temperature ◽  
Relative Standard

Objective: The main objective of present study was to Isolate, characterize and validate a reverse phase high performance liquid chromatographic method was validated for quantification of bis-[10-(2-methyl-4H-3-thia-4,9-diazabenzo[f]azulene)]-1,4-piperazine in Olanzapine drug substance; it decreases the mental disorders in human body. The method is specific, rapid, precise and accurate for the separation and determination of bis-[10-(2-methyl-4H-3-thia-4,9-diazabenzo[f]azulene)]-1,4-piperazine in Olanzapine drug substance form.Methods: The bis-[10-(2-methyl-4H-3-thia-4,9-diazabenzo[f]azulene)]-1,4-piperazine of Olanzapine was resolved on a Zorbax RX-C 8, 250 mm X 4.6 mm, 5 micron column (L-1) using a mobile phase system containing 0.03 M sodium dodecyl sulphate in water pH 2.5 with 1 N sodium hydroxide solution and acetonitrile in the ratio of (Mobile phase A-52:48 v/v) and (Mobile phase B-buffer and Acetonitrile 30:70 v/v) by using the gradient program. The mobile phase was set at a flow rate of 1.5 ml/min and the volume injected was 20μl for every injection. The detection wavelength was set at 220 nm and the column temperature was set at 35 °C.Results: The proposed method was productively applied for the quantitative determination of bis-[10-(2-methyl-4H-3-thia-4,9-diazabenzo [f]azulene)]-1,4-piperazine in Olanzapine drug substance form. The linear regression analysis data for calibration plots showed a good linear relationship over a concentration range of 0.025to 0.903 µg/ml for bis-[10-(2-methyl-4H-3-thia-4,9-diazabenzo[f]azulene)]-1,4-piperazine, 0.081-0.608 µg/ml for Olanzapine. The mean values of the correlation coefficient were 0.999 and 0.999 for bis-[10-(2-methyl-4H-3-thia-4,9-diazabenzo[f]azulene)]-1,4-piperazine and Olanzapine. The method was validated as per the ICH guidelines. The detection limit (LOD) was about 0.007 µg/ml, 0.024 µg/ml and quantitation limit (LOQ) was about 0.024 µg/ml, 0.081 µg/ml for bis-[10-(2-methyl-4H-3-thia-4,9-diazabenzo[f]azulene)]-1,4-piperazine and Olanzapine. The relative standard deviation was found to be 1.64 % and 2.18 % for bis-[10-(2-methyl-4H-3-thia-4,9-diazabenzo[f]azulene)]-1,4-piperazine and Olanzapine.Conclusion: The validated HPLC method and the statistical analysis showed that the method is repeatable and selective for the estimation of the bis-[10-(2-methyl-4H-3-thia-4,9-diazabenzo[f]azulene)]-1,4-piperazine of the Olanzapine drug substance.

A conductivity detector for liquid chromatography with a cell volume of 0.1 μl

1983 ◽  
Vol 48 (4) ◽  
pp. 1129-1136 ◽  
Author(s):  
Danuše Kouřilová ◽  
Karel Šlais ◽  
Miloš Krejčí
Keyword(s):  
Liquid Chromatography ◽  
Organic Acids ◽  
Cell Volume ◽  
Mobile Phase ◽  
Linear Range ◽  
Phase System ◽  
Reverse Phase ◽  
Micropacked Columns ◽  
A Cell ◽  
Inner Diameter

A conductivity detector with a cell volume of 0.1 μl has been devised to fit glass micropacked columns with an inner diameter of 0.5 mm. D.c. current was used in the measurements, the voltage applied to the electrodes was 30 V. Organic acids separated in a reverse-phase system were detected; the minimum detectable concentrations were 6 . 10-7 - 1 . 10-5 mol l-1 according to the acid concerned and the composition of the mobile phase. The linear range of the detector is 400.

scholarly journals Application of Hydrophilic Interaction Liquid Chromatography for the Quantification of Flavonoids inGenista tinctoriaExtract

2016 ◽  
Vol 2016 ◽  
pp. 1-9 ◽  
Author(s):  
Aleksandra Sentkowska ◽  
Magdalena Biesaga ◽  
Krystyna Pyrzynska
Keyword(s):  
Mobile Phase ◽  
Retention Mechanism ◽  
Chromatographic Behavior ◽  
Hydrophilic Interaction ◽  
Silica Column ◽  
Retention Factors ◽  
Component Content ◽  
Chromatographic Procedure ◽  
Unmodified Silica ◽  
Genista Tinctoria

Hydrophilic interaction chromatography (HILIC) was employed to investigate chromatographic behavior of selected flavonoids from their different subgroups differing in polarity. Chromatographic measurements were performed on two different HILIC columns: unmodified silica (Atlantis-HILIC) and zwitterionic sulfoalkylbetaine (SeQuant ZIC-HILIC). Separation parameters such as content and type of organic modifier were studied. On ZIC column retention factors were observed to be inversely proportional to the buffer content in the mobile phase, which is the typical partitioning mechanism. In the case of bare silica column more or less apparent dual retention mechanism was observed, depending on the water component content in the mobile phase. ZIC-HILIC showed better selectivity (in comparison to silica column) with the detection limit of 0.01 mg/L (only for rutin was 0.05 mg/L). Finally, this chromatographic procedure was validated and applied for the determination of some flavonoids inGenista tinctoriaL. extract.

scholarly journals Fast HPLC Method Using Ion-Pair and Hydrophilic Interaction Liquid Chromatography for Determination of Phenylephrine in Pharmaceutical Formulations

2010 ◽  
Vol 93 (5) ◽  
pp. 1436-1442 ◽  
Author(s):  
Michal Douòa ◽  
Petr Gibala
Keyword(s):  
Liquid Chromatography ◽  
Fluorescence Detection ◽  
Flow Rate ◽  
Mobile Phase ◽  
Hplc Method ◽  
Ion Pair ◽  
Hydrophilic Interaction Liquid Chromatography ◽  
Hydrophilic Interaction ◽  
Injection Volume ◽  
Ion Pair Chromatography

Abstract A rapid procedure based on a direct extraction and HPLC determination with fluorescence detection of phenylephrine in pharmaceutical sachets that include a large excess of paracetamol (65 + 1, w/w), ascorbic acid (5 + 1, w/w), and other excipients (aspartame and sucrose) was developed and validated. The final optimized chromatographic method for ion-pair chromatography used an XTerra RP18 column, 3 µm particle size, 50 ⨯ 3.0 mm id. The mobile phase consisted of a mixture of acetonitrile and buffer (10 mM sodium octane-1-sulfonate, adjusted with H3PO4 to pH 2.2; 200 + 800, v/v), with a constant flow rate of 0.3 mL/min. The separation was carried out at 30C, and the injection volume was 3 µL. Fluorescence detection was performed at excitation and emission wavelengths of 275 and 310 nm, respectively. The mobile phase parameters, such as the organic solvent fraction (acetonitrile) in mobile phase as an organic modifier, the concentration of sodium octane-1-sulfonate as a counter-ion, temperature, and pH of mobile phase, were studied. As an alternative to ion-pair chromatography, hydrophilic interaction liquid chromatography (HILIC) was investigated using a Luna HILIC column, 3 m, 100 ⨯ 4.6 mm id. The mobile phase consisted of acetonitrile and buffer (5 M potassium dihydrogen phosphate, adjusted with H3PO4 to pH 2.5; 750 + 250, v/v) at a flow rate of 0.8 mL/min. The separation was carried out at 25°C, and the injection volume was 5 µL. The proposed method has an advantage of a very simple sample pretreatment, and is much faster than the currently utilized HPLC methods using gradient elution and UV detection. Commercial samples of sachets were successfully analyzed by the proposed HPLC method.

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