Asian Journal of Research in Chemistry

Tentu Nageswara Rao ¹, Muralidhar Reddy Avuthu ², B. Venkata Reddy ³, S. N. V. S. Murthy ⁴

Affiliations
1 Department of Chemistry, Krishna University, Machilipatnam, A.P., IN
2 Department of Chemistry, SVKP & Dr. K.S Raju Arts & Science College, Penugonda, A.P, IN
3 Department of Animal Science, Chonbuk National University, Jeonju, KP
4 Department of Chemistry, DLR PG College, G. Mamidada, AP, IN

Abstract

A simple and inexpensive method was developed with high performance liquid chromatography with PDA detection for determination of Terbinafine HCl and related impurities. The chromatographic separations were achieved on (150×4.6 mm), 5.0 μm make: YMC-Pack ODS-AM, 120A column employing Acetonitrile: methanol and Water pH 7.5, in the ratio of 20:10:10 v/v/v as mobile phase with gradient programmed at flow rate 1.0 mL/min was chosen. Three impurities were eluted within 35 minutes. The detector wavelength of 230 nm was employed.

Keywords

Forced Degradation, HPLC, Method Validation, Terbinafine.

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Tentu Nageswara Rao ¹, Botsa Parvatamma ², Karri Apparao ¹, Jakka Mastan ¹

Affiliations
1 Department of Chemistry, Krishna University, Machilipatnam, Andhra Pradesh, IN
2 Department of Organic Chemistry, Gayathri PG College, Vizianagaram, Andhra Pradesh, IN

Abstract

A simple and inexpensive method was developed using solid-phase extraction, together with gas chromatographic method and high performance liquid chromatographic method for determination of chlorpyrifos and its metabolite O,O-diethyl triphosphate residues in green apples. The evaluated parameters include the extracts by silica gel packed column using methanol and water solvent mixture (90:10) and ethyl acetate solvents. The method was validated using green apple fruit samples spiked with chlorpyrifos and its metabolite (O,O-diethyl triphosphate) at different fortification levels (0.01 and 0.1 mg/kg). Average recoveries (using each concentration six replicates) of range 86-95%. The calibration solutions concentration in the range 0.01-5.0 mg/L and limit of detection (LOD) and limit of quantification (LOQ) were 0.003 mg/kg and 0.01 mg/kg respectively. Finally the green apple fruit residue samples were analyzed by GC and HPLC.

Keywords

HPLC, GC, Silica Gel, Chlorpyrifos, O,O-Diethyl Triphosphate and Green Apples.

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