scholarly journals GC-MS/MS method for simultaneous determination of ester forms of 3-MCPD and 2-MCPD in infant formula

2020 ◽  
Vol 3 (2) ◽  
pp. 133-144
Author(s):  
Chi Le Dinh ◽  
Thuong Nguyen Nhu ◽  
Tu Vu Ngoc ◽  
Hong Hao Le Thi ◽  
Son Tran Cao ◽  
...  
Keyword(s):  
Sulfuric Acid ◽  
Infant Formula ◽  
Flow Rate ◽  
Mobile Phase ◽  
Capillary Column ◽  
Phenylboronic Acid ◽  
Tandem Mass ◽  
Internal Standards ◽  
Product Ions

A sensitive GC-MS/MS method has been developed and validated for determining ester forms of 3-MCPD and 2-MCPD in infant formula, using 3-MCPD-d5 and 2-MCPD-d5 as internal standards, respectively. The esters of MCPDs were extracted from infant formula powder with mixture of ethanol/n-hexane/diethyl ether (1/1/1, v/v/v), then treated with sulfuric acid to release free MCPDs. Free MCPDs and internal standards were derivatized with phenylboronic acid and the corresponding derivatives were used for GC-MS/MS analysis. The chromatographic separation was performed in a DB-5MS capillary column using helium as mobile phase at flow rate of 1 mL/min. Tandem mass spectroscopic detection of each analyte was done in MRM mode by monitoring one precursor ion and two product ions. Validation results confirmed the suitability of the developed method for intended application. Application of the method in samples collected from different provinces in Vietnam detected esterified 3-MCPD in 38.9% of samples, esterified 2-MCPD in 34.7% of samples.

Optimum HPLC Conditions for Determination of Dibucaine HCL, Fluocortolone Pivalate and Fluocortolone Caproate by Using Experimental Design

2018 ◽  
Vol 15 (1) ◽  
pp. 32-38 ◽  
Author(s):  
Bürge Aşçı ◽  
Mesut Koç
Keyword(s):  
Experimental Design ◽  
Flow Rate ◽  
Mobile Phase ◽  
High Performance ◽  
Limit Of Detection ◽  
Pharmaceutical Preparations ◽  
Acid Mixture ◽  
Solution Stability ◽  
Uv Detector

Introduction:This paper presents the development and validation of a novel, fast, sensitive and accurate high performance liquid chromatography (HPLC) method for the simultaneous quantitative determination of dibucaine HCl, fluocortolone pivalate and fluocortolone caproate in pharmaceutical preparations.Experiment:Development of the chromatographic method was based on an experimental design approach. A five-level-three-factor central composite design requiring 20 experiments in this optimization study was performed in order to evaluate the effects of three independent variances including mobile phase ratio, flow rate and amount of acid in the mobile phase.Conclusion:The optimum composition for mobile phase was found as a methanol:water:acetic acid mixture at 71.6 : 26.4 : 2 (v/v/v) ratio and optimum separation was acquired by isocratic elution with a flow rate of 1.3 mL/min. The analytes were detected using a UV detector at 240 nm. The developed method was validated in terms of linearity, precision, accuracy, limit of detection/quantitation and solution stability and successfully applied to the determination of dibucaine HCl, fluocortolone pivalate and fluocortolone caproate in pharmaceutical topical formulations such as suppositories and ointments.

scholarly journals Box-Behnken Assisted Validation and Optimization of an RP-HPLC Method for Simultaneous Determination of Domperidone and Lansoprazole

Separations ◽  
2021 ◽  
Vol 8 (1) ◽  
pp. 5
Author(s):  
Mohd Afzal ◽  
Mohd. Muddassir ◽  
Abdullah Alarifi ◽  
Mohammed Tahir Ansari
Keyword(s):  
Flow Rate ◽  
Mobile Phase ◽  
Limit Of Detection ◽  
Hplc Method ◽  
Box Behnken Design ◽  
Rp Hplc ◽  
System Suitability ◽  
Method Optimization ◽  
Key Variables

A highly specific, accurate, and simple RP-HPLC technique was developed for the real-time quantification of domperidone (DOMP) and lansoprazole (LANS) in commercial formulations. Chromatographic studies were performed using a Luna C8(2), 5 μm, 100Å, column (250 × 4.6 mm, Phenomenex) with a mobile phase composed of acetonitrile/2 mM ammonium acetate (51:49 v/v), pH 6.7. The flow rate was 1 mL·min−1 with UV detection at 289 nm. Linearity was observed within the range of 4–36 µg·mL−1 for domperidone and 2–18 µg·mL−1 for lansoprazole. Method optimization was achieved using Box-Behnken design software, in which three key variables were examined, namely, the flow rate (A), the composition of the mobile phase (B), and the pH (C). The retention time (Y1 and Y3) and the peak area (Y2 and Y4) were taken as the response parameters. We observed that slight alterations in the mobile phase and the flow rate influenced the outcome, whereas the pH exerted no effect. Method validation featured various ICH parameters including linearity, limit of detection (LOD), accuracy, precision, ruggedness, robustness, stability, and system suitability. This method is potentially useful for the analysis of commercial formulations and laboratory preparations.

scholarly journals RP-HPLC Determination of Raloxifene in Pharmaceuticl Tablets

2006 ◽  
Vol 3 (1) ◽  
pp. 60-64 ◽  
Author(s):  
P. Venkata Reddy ◽  
B. Sudha Rani ◽  
G. Srinu Babu ◽  
J. V. L. N. Seshagiri Rao
Keyword(s):  
Flow Rate ◽  
Retention Time ◽  
Mobile Phase ◽  
Dosage Forms ◽  
Hplc Method ◽  
Reverse Phase Hplc ◽  
Reverse Phase ◽  
Pharmaceutical Dosage Forms ◽  
Rp Hplc

A reverse phase HPLC method is developed for the determination of Raloxifene in pharmaceutical dosage forms. Chromatography was carried out on an inertsil C18 column using a mixture of acetonitrile and phosphate buffer (30:70 v/v) as the mobile phase at a flow rate of 1 mL/min. Detection was carried out at 290 nm .The retention time of the drug was 10.609 min. The method produced linear responses in the concentration range of 0.5-200 µg/mL of Raloxifene. The method was found to be applicable for determination of the drug in tablets.

scholarly journals Measurement of Urinary d- and l-2-Hydroxyglutarate Enantiomers by Stable-Isotope-Dilution Liquid Chromatography–Tandem Mass Spectrometry after Derivatization with Diacetyl-l-Tartaric Anhydride

2004 ◽  
Vol 50 (8) ◽  
pp. 1391-1395 ◽  
Author(s):  
Eduard A Struys ◽  
Erwin E W Jansen ◽  
Nanda M Verhoeven ◽  
Cornelis Jakobs
Keyword(s):  
Mass Spectrometry ◽  
Differential Diagnosis ◽  
Liquid Chromatography ◽  
Stable Isotope ◽  
Tandem Mass Spectrometry ◽  
Tandem Mass ◽  
Internal Standards ◽  
Chromatography Tandem Mass Spectrometry ◽  
Liquid Chromatography Tandem Mass

Abstract Background: The differential diagnosis of d-2-hydroxyglutaric aciduria (d-2-HGA), l-2-hydroxyglutaric aciduria (l-2-HGA), and the combined d/l-2-hydroxyglutaric aciduria (d/l-2-HGA) can be accomplished only by the measurement of the corresponding 2-hydroxyglutarate (2-HG). Available methods for the determination of d- and l-2-HG in urine are either time-consuming and expensive or have not been extensively validated. We aimed to develop a method for their rapid and sensitive measurement. Methods: We used liquid chromatography–tandem mass spectrometry (LC-MS/MS) for the determination of d- and l-2-HG with stable-isotope-labeled internal standards. Urine samples of 20 μL were mixed with 250 μL of methanol containing the internal standards and subsequently dried under nitrogen. The analytes were derivatized by use of diacetyl-l-tartaric anhydride (DATAN) to obtain diastereomers, which were separated on an achiral C18 HPLC column and detected by MS/MS in multiple-reaction-monitoring mode. Results: The use of DATAN as chiral derivatization reagent provided very well separated peaks of the formed diastereomers of d- and l-2-HG, with a total runtime of 5 min. The inter- and intraassay CVs for d- and l-2-HG ranged from 3.4% to 6.2%. Mean recoveries of d- and l-2-HG, evaluated on two concentrations, were 94%. Detection limit of the presented method was 20 pmol for a sample volume of 20 μL. Method comparison of the LC-MS/MS method with a gas chromatography–mass spectrometry method, in which d- and l-2-HG were derivatized with R-(−)-butanol, showed good agreement between the two methods. Conclusions: Urinary d- and l-2-HG can be analyzed by MS/MS after derivatization with DATAN. The presented method may be suitable for the differential diagnosis of 2-HGA.

scholarly journals Direct Determination of Free Methionine in Soy-Based Infant Formula

2004 ◽  
Vol 87 (1) ◽  
pp. 123-128
Author(s):  
Paul Johns ◽  
Rosalyn Phillips ◽  
Lobat Dowlat
Keyword(s):  
Infant Formula ◽  
Mobile Phase ◽  
Method Comparison ◽  
Water System ◽  
Direct Determination ◽  
Reversed Phase ◽  
Intermediate Precision ◽  
Relative Standard ◽  
Limit Of Quantitation

Abstract A method was developed for the direct determination of free methionine in soy-based infant formula, with analyte separation and quantitation by reversed-phase liquid chromatography (LC), and UV absorbance at 214 nm, respectively. Sample preparation required only dilution with mobile phase and syringe filtration. Using a 0.02M KH 2 PO 4 mobile phase (pH adjusted to 2.9 with 85% o-phosphoric acid) and 0.7 mL/min flow rate, methionine eluted at approximately 8 min, and total run time was 14 min after column regeneration with acetonitrile–water. System linearity was demonstrated as peak area versus analyte concentration, ranging from 80 to 120% of the formula specification for free methionine (r > 0.999, and all residuals <0.45%). Intermediate precision relative standard deviation values were <1.5% for ready-to-feed and reconstituted powder samples, and recoveries ranged from 98.0 to 103.5% for inter-method comparison with an amino acid analyzer method. The limit of quantitation was 3 mg methionine/L in the “as fed” infant formula. Despite the relatively weak UV absorptivity of methionine, the 214 nm signal was sufficiently intense in the 30–65 mg/L (201–436 μM) range to afford quantitation by peak area proportionation versus a 2-point external standard calibration. This direct UV detection after reversed-phase LC separation provides a simple and accurate method for determining free methionine without derivatization.

scholarly journals Validated Stability-Indicating HPLC-UV Method for Simultaneous Determination of Glipizide and Four Impurities

2011 ◽  
Vol 94 (2) ◽  
pp. 523-530 ◽  
Author(s):  
Sakshi Gupta ◽  
Gulshan Bansal
Keyword(s):  
Simultaneous Determination ◽  
Flow Rate ◽  
Retention Time ◽  
Mobile Phase ◽  
Stability Testing ◽  
Stability Indicating ◽  
Chromatographic Parameters ◽  
Interday Precision ◽  
Calculated Amount

Abstract A selective stability-indicating HPLC-UV method for simultaneous determination of glipizide and four impurities (DPs IIV) formed under hydrolytic conditions was developed and validated. The drug and impurities were resolved on an XTerra C18 column (250 4.5 mm id) in a single gradient run using buffer (0.005 M KH2PO4; pH 3.0)methanol (60 40, v/v; mobile phase A) and (20 80, v/v; mobile phase B) at a flow rate of 0.5 mL/min with 230 nm detection wavelength. The method was linear across concentration ranges of 0.2100, 0.1100, 0.5100, 0.2100, and 0.150 0000g/mL for glipizide and DPs IIV, respectively. The RSD for intraday and interday precision for the drug and impurities was <1 and <1.2, respectively. Satisfactory recoveries (96.5899.97) of each of the three concentrations selected across the linearity range of each analyte were obtained, proving the method was sufficiently accurate. The LOD was 0.07, 0.05, 0.16, 0.08, and 0.05 g/mL and the LOQ was 0.20, 0.14, 0.50, 0.23, and 0.14 g/mL for the drug and DPs IIV, respectively. Each peak was resolved with resolution of >2 from the nearest peak. Insignificant changes in retention time (<4) and calculated amount (<1.65) of drug and each impurity upon small but deliberate changes in various chromatographic parameters were observed, suggesting the method was robust. The method was applied successfully to stability testing of glipizide tablets.

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