scholarly journals ANALYTICAL METHOD DEVELOPMENT BY SOLID PHASE EXTRACTION AND HIGH-PERFORMANCE LIQUID CHROMATOGRAPHY FOR DIPHENHYDRAMINE QUANTIFICATION IN SYRUPS

2017 ◽  
Vol 9 (6) ◽  
pp. 106
Author(s):  
Marcela Hurtado ◽  
Jose Raul Medina
Keyword(s):  
Solid Phase Extraction ◽  
High Performance ◽  
Method Development ◽  
Solid Phase ◽  
Reversed Phase ◽  
Phase Extraction ◽  
Diphenhydramine Hydrochloride ◽  
Liquid Liquid Extraction ◽  
Validation Parameters

Objective: To develop a method for the determination of diphenhydramine hydrochloride in syrups.Methods: The developed method is based on the active ingredient recovery from the pharmaceutical formulation using a cartridge for selective solid phase extraction. This procedure is simple and fast as compared to the methods that require liquid/liquid extraction. Once the sample is eluted from the cartridge, it is injected directly into a reversed-phase chromatographic system containing a mixture of acetonitrile: 10 mmol ammonium acetate: triethylamine 60:39.5:0.5.Results: The proposed method fulfilled the validation parameters (linearity R2>0.99, precision CV<2% and accuracy 98-102%).Conclusion: The proposed method proved to be reliable when it was applied in the quantification of diphenhydramine hydrochloride of two commercial syrup products.

scholarly journals Determination of Flumorph Residues in Vegetables, Soil, and Natural Water by Solid-Phase Extraction Cleanup and High-Performance Liquid Chromatography with UV Detection

2008 ◽  
Vol 91 (6) ◽  
pp. 1459-1466 ◽  
Author(s):  
Ji-Ye Hu ◽  
Yu-Chao Zhang ◽  
Hai Yan
Keyword(s):  
Solid Phase Extraction ◽  
Natural Water ◽  
High Performance ◽  
Solid Phase ◽  
Residue Analysis ◽  
Reversed Phase ◽  
Uv Detection ◽  
Phase Extraction ◽  
Limit Of Quantification

Abstract A method for high-performance liquid chromatographic (HPLC) determination of flumorph residues in cucumber, tomato, soil, and natural water was developed and validated. Primary secondary amine or octadecylsilyl (C18) solid-phase extraction cartridges were used for sample preparation. Reversed-phase HPLC with UV detection was used for separation and quantification of the pesticide. The combined cleanup and chromatographic method steps were sensitive and reliable for simultaneous determination of residues of the 2 isomers of flumorph in the studied samples. This method is characterized by recovery &gt;97.9, coefficient of variation &lt;6.2, and limit of quantification of 0.01 mg/kg, in agreement with directives for method validation in residue analysis. Flumorph residues in the samples were further confirmed by HPLC/mass spectrometry. The proposed method is fast, easy to perform, and could be used for monitoring of pesticide residues.

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