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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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G. Kumar ¹, T. B. Patrudu ², Tentu Nageswara Rao ¹, M. V. Basaveswara Rao ¹

Affiliations
1 Department of Chemistry, Krishna University, Machilipatnam, A.P., IN
2 Department of Chemistry, GITAM University, Hyderabad Campus, Telangana, IN

Abstract

A simple and inexpensive method was developed with high performance liquid chromatography with PDA detection for determination of entacapone and its related impurities are (N, N diethyl cyano acetamide), (3,4 Dihydroxy 5-Nitro benzaldehyde) and (2-Z)-2-Cyano-3-(3,4-Dihydroxy-5-nitrophenyl)N,N-diethyl-2- propenamide. The chromatographic separations were achieved on (250×4.6 mm), 5.0 μm make: Phenomenex Luna column employing Acetonitrile: HPLC Water in the ratio of 50:50 (v/v) as mobile phase with isocratic at flow rate 0.9 mL/min was chosen. Three impurities were eluted within 15 minutes. The column temperature was maintained at 30°C and a detector wavelength of 210 nm was employed. The method was successfully validated by establishing System Suitability, Specificity, Linearity, Accuracy, limit of detection and Limit of quantification.

Keywords

HPLC, Method Validation, Related Impurities, Entacapone, LOQ, LOD.

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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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Botsa Parvatamma ¹, Tentu Nageswara Rao ², T. B. Patrudu ³, Karri Apparao ¹

Affiliations
1 Department of Organic Chemistry, Gayathri PG College, Vizianagaram, Andhra Pradesh, IN
2 Department of Chemistry, Krishna University, Machilipatnam, Andhra Pradesh, IN
3 Department of Chemistry, Gitam University, Hyderabad Campus, Telangana, IN

Abstract

A simple and inexpensive method was developed with high performance liquid chromatography with PDA detection for determination of Fosinopril Sodium and its related impurities. The chromatographic separations were achieved on (250×4.6 mm), 3.0 μm make: Hypersil ODS column employing HPLC Water: Acetonitrile:1% orthophosphoric acid in water in the ratio of 65:25:10 (v/v/v) as mobile phase initially with gradient run and flow rate set as 1.2 mL/min was chosen. Time/A/B: Time/A/B/C: 30/50/40/10; 35/50/40/10; 45/35/55/10; 80/35/55/10; 90/65/25/10; 100/65/25/10. All impurities were eluted within 60 minutes. The column temperature was maintained at 35°C and a detector wavelength of 210 nm was employed. The method was successfully validated by establishing System Suitability, Specificity, Linearity, Precision, Accuracy, Limit of detection and Limit of quantification.

Keywords

HPLC, Method Validation, Related Impurities, Fosinopril Sodium, LOQ, LOD.

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Tentu Nageswara Rao ¹, A. Vijayalakshmi ², Karri Apparao ¹, N. Krishnarao ¹

Affiliations
1 Department of Chemistry, Krishna University, Machilipatnam, Andhra Pradesh, IN
2 Department of Marine Living Resources, Andhra University, Visakhapatnam, Andhra Pradesh, IN

Abstract

A simple and inexpensive method was developed with high performance liquid chromatography with PDA detection for determination of olmesartan Medoxomil and its related impurities. The chromatographic separations were achieved on (250×4.6 mm), 5.0 μm make: Zorbax Eclipse XDB-C8 column employing 00.1% H3PO4 in Water: Acetonitrile in the ratio of 50:50 (v/v) as mobile phase with gradient initially A:B:70:30 and followed as Time/A/B: 25/30/70; 30/30/70; 31/75/25 and runtime is 35 mins at flow rate 1.0 mL/min was chosen. All impurities were eluted within 18 minutes. The column temperature was maintained at 30oC and a detector wavelength of 225 nm was employed. The method was successfully validated by establishing Specificity, Linearity, Precision, Accuracy, Limit of detection and Limit of quantification.

Keywords

HPLC, Method Validation, Related Impurities, Olmesartan Medoxomil, LOQ, LOD.

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Tentu Nageswara Rao ¹, Karri Apparao ¹, N. Krishnarao ¹, A. Vijayalakshmi ²

Affiliations
1 Department of Chemistry, Krishna University, Machilipatnam, Andhra Pradesh, IN
2 Department of Marine Living Resources, Andhra University, Visakhapatnam, Andhra Pradesh, IN

Abstract

A simple and inexpensive method was developed with high performance liquid chromatography with PDA detection for determination of benazepril hydrochloride and its related impurities. The chromatographic separations were achieved on (250×4.6 mm), 5.0 μm make: Symmetry Shield column employing 0.02M tetrabuthylammonium hydroxide + 0.05 % v/v acetic acid : methanol in the ratio of 50:50 (v/v) as mobile phase with isocratic at flow rate 1.0mL/min was chosen. All impurities were eluted within 30 minutes. The column temperature was maintained at 25°C and a detector wavelength of 240 nm was employed. The method was successfully validated by establishing System Suitability, Specificity, Linearity, Precision, Accuracy, Limit of detection and Limit of quantification.

Keywords

HPLC, Method Validation, Related Impurities, Benazepril Hydrochloride, LOQ, LOD.

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