Active Ingredient Estimation of Clopyralid Formulation by Reversed Phase HPLC

Singh A Tandon S

doi:10.4172/2157-7064.1000257

Abstract

A simple, accurate, and reliable high-performance liquid chromatography (HPLC) method was developed for determination, separation and estimation of clopyralid active ingredient in its formulation. The active ingredient in formulation was estimated by two methods and cleanup was performed using C18 SPE. Estimation was done by HPLC using 5 μm, C18 column, and mobile phase 0.02 % acetic acid in methanol: acetonitrile (90:10 v/v) and detection at 229 nm. The efficiency of clean up for standard clopyralid was found to be 98.02-98.66% at different concentrations. Overall recoveries for different methods ranged from 98.3-100.1 %. The LOD and LOQ were 0.1 and 0.3 ng respectively. The detector response was linear within concentrations range 0.25-10.0 ng at RSD 1.87%.

Highlights

Pesticides are indispensable for sustained agricultural production
In order to check passage of spurious/sub-standard formulation to the consumer to save him from avoidable losses from pests, it is necessary to develop a convenient and reliable method of estimation of active ingredient in a formulation
Validation: The method was validated by evaluating it in terms of specificity, linearity, precision, accuracy, Limit of Detection (LOD) and Limit of Quantification (LOQ)

Summary

Introduction

Pesticides are indispensable for sustained agricultural production. The successful employment of any pesticide depends upon stabilities of its formulation. As per our literature search, no method has been reported for the estimation of clopyralid in its formulation using SPE method and determination by RP-HPLC. (2014) Active Ingredient Estimation of Clopyralid Formulation by Reversed Phase HPLC. First method involved preparation of 100 ppm stock solution by dissolving 0.1 mL of formulation (clopyralid 10% SL) in 100 mL of distilled water. From this solution serial dilution of 10, 5, 2, 1, and 0.5 ppm were made. Diluted solution (2, 1 and 0.5 ppm) of formulation was loaded (0.5 mL) on cartridge and washed with 2 mL water followed by 1 mL methanol and washings was discarded eluted with 2 mL methanol. Validation: The method was validated by evaluating it in terms of specificity, linearity, precision, accuracy, Limit of Detection (LOD) and Limit of Quantification (LOQ)

Results and Discussion

Method validation

Conclusion

Method used Standard pure compound