Liquid Chromatography With UV Detection For Simultaneous Determination Of Ciprofloxacin And Metronidazole

2014 ◽  
Vol 72 (1) ◽  
Author(s):  
Agnes Budiarti ◽  
Ibnu Gholib Gandjar ◽  
Abdul Rohman

The aim of this study was to develop HPLC method capable of facilitating the simultaneous determination of ciprofloxacin hydrochloride (CIP.HCl) and metronidazole (MDZ). The analytes were separated with Lichrospher 100 RP-18 C18 column (100 x 4.6 mm, 5 μm). The mobile phase consisted of monobasic potassium phosphate (50 mM, pH 3.5) and acetonitrile (80: 20, v/v) containing triethylamine (7.5 mM) delivered isocratically with flow rate of 1.0 mL/min. The UV detection was set 298 nm. The developed method was validated in terms of precision, accuracy, linearity, selectivity and sensitivity. The precision of the method was evaluated using repeatability assay which RSD values of 0.37 – 1.72 % and 0.10 – 1.90 % for CIP.HCl and MDZ, respectively. The mean recoveries of CIP.HCl and MDZ were 99.83 – 100.77% and 99.80 – 101.14%, respectively. The dynamic linear response exhibited good correlation (r > 0.99) within the concentration range of 30 – 90 µg/mL for both drugs. The proposed method has been successfully applied for the simultaneous determination of CIP.HCl and MDZ in tablet dosage forms.

2010 ◽  
Vol 93 (4) ◽  
pp. 1086-1092 ◽  
Author(s):  
Anna Gumieniczek ◽  
Anna Berecka ◽  
ukasz Komsta

Abstract For type 2 diabetes treatment, combinations of drugs from the thiazolidinedione and sulfonylurea groups are now available in the same tablet or capsule. Therefore, a stability-indicating and validated HPLC method was developed for simultaneous determination of pioglitazone, rosiglitazone, and glipizide in combined dosage forms. The examined drugs were subjected to different conditions such as acid and base, temperature, and UV light, and degradation of pioglitazone and glipizide was observed under thermal and acidic stress. However, selectivity of the presented method for pioglitazone, rosiglitazone, and glipizide assay against their degradation products was confirmed. It was also demonstrated to be robust, resisting small deliberate changes in pH of the buffer, flow rate, and percentage of acetonitrile in the mobile phase. The presented method utilizes a LiChrospher RP18 column (125 4.0 mm), acetonitrile in phosphate buffer at pH 4.3 (40 + 60, v/v) as the mobile phase, and UV detection at 225 nm for pioglitazone/glipizide or 245 nm for rosiglitazone/glipizide. The method was validated with respect to linearity, precision, and accuracy. Finally, the elaborated procedure was applied for the QC of pioglitazone/glipizide and rosiglitazone/glipizide mixtures.


INDIAN DRUGS ◽  
2016 ◽  
Vol 53 (09) ◽  
pp. 42-46
Author(s):  
M Debnath ◽  
◽  
A. S. Kumar ◽  
V. D. S Ganta

A simple and precise RP‐HPLC method was developed and validated for the determination of pioglitazone hydrochloride in pharmaceutical dosage forms. Chromatography was carried out using Kromosil- C18 ODS column (250 x 4.6 mm; 5 μm), mixture of acetate buffer: methanol (40:60 v/v) as the mobile phase at a flow rate 1.0 mL/min. The analyte was monitored using UV detector at 254 nm. The retention time for pioglitazone HCl was 3.063 min. The proposed method was found linear in the concentration range of 20.0‐70.0 μg/ml with correlation coefficient of r2=0.9999. The developed method has been statistically validated and found simple and accurate. The mean recoveries obtained for pioglitazone HCl were in the range 99.20-101.59%. Due to its simplicity, rapidness, high precision and accuracy of the proposed method it may be used for determining pioglitazone HCl in bulk and dosage forms.


Author(s):  
N V Fares ◽  
Haitham A El Fiky ◽  
Amr M Badawey ◽  
Maha F Abd El Ghany

Abstract Background Validated UPLC method and TLC densitometric method were prescribed for determination of antihypertensive components. Objectives: To establish and validate rapid and accurate Ultra performance liquid chromatographic (UPLC) and TLC densitometric methods for determination of Xipamide and Triamterene in pure and dosage forms. Methods The first method; UPLC method, depended on using Agilent Zorbax Eclipse Plus C8 (50 mm × 2.1 mm, 1.8 μm), as the column, mobile phase composed of (acetonitrile-water) (70 + 30, v/v) adjusted by acetic acid to obtain (pH 3), 0.2 mL/min flow rate and UV detection at 231.4 nm. The second method was a thin layer chromatography (TLC) densitometric method, separation was achieved by using toluene-methanol-ethyl chloride-acetic acid (7 + 2 + 1 + 0.2, v/v/v) as the mobile phase, pre coated silica gel plates as the stationary phase and UV detection at 300.0 nm. Results The obtained results were validated and statistically compared with official and reported methods. The obtained results showed high accuracy and reproducible results with excellent mean recoveries for both drugs. Conclusions The UPLC method showed shorter retention time for both Xipamide (0.88 min) and Triamterene (0.63 min), lower detection limit less than 0.055 µg/mL for both drugs with high selectivity, decreased injection volume (1 µL) and lower flow rate other than any HPLC method. Both proposed methods were sensitive, selective, and effectively applied to pure and dosage forms (Epitens®). Highlights Unprecedented sensitive, rapid, and reproducible UPLC and TLC methods were developed for selective determination of mixture of Xipamide and Triamterene with LOD less than 0.076 µg/mL for both drugs.


INDIAN DRUGS ◽  
2013 ◽  
Vol 50 (03) ◽  
pp. 26-29
Author(s):  
J. J Jadhav ◽  
◽  
S Mungekar ◽  
J. V. Velada ◽  
H. A. Doshi ◽  
...  

A simple, sensitive, precise and specific normal phase high performance liquid chromatography (HPLC) method was developed and validated for the determination of dimethicone from tablet dosage forms. It was found that the excipients used in the tablet dosage form did not interfere in the quantification of dimethicone. The HPLC separation was carried out by normal phase chromatography on Princeton Sphere Cyano, 250 x 4.6mm, 5µ with a mobile phase composed of hexane : ethanol : ethyl acetate (80:20:0.2) in isocratic mode at a flow rate of 0.5mL/min. Dimethicone was quantified using a refractive index detector. The calibration curve for dimethicone was linear from 1.75 to 3.25 mg/mL. The inter-day and intra-day precisions were found to be within limits. The proposed method has adequate sensitivity, reproducibility and specificity for the determination of dimethicone from tablet dosage forms.


2011 ◽  
Vol 94 (4) ◽  
pp. 1089-1093 ◽  
Author(s):  
Fernando Henrique Andrade Nogueira ◽  
Letícia De Paula Lana Goulart ◽  
Isabela Da Costa César ◽  
Lígia Maria Moreira De Campos ◽  
Gérson Antônios Pianetti

Abstract A simple HPLC method for determination of mefloquine hydrochloride in tablets was developed and validated. The separation was carried out on an Xterra RP18 (250 × 4.6 mm id, 5 µm particle size) analytical column. The mobile phase was 0.05 M monobasic potassium phosphate buffer (pH 3.5)–methanol (40 + 60, v/v). The flow rate and wavelength were set to 1 mL/min and 283 nm, respectively. The method was specifc for mefloquine hydrochloride in the presence of hydrolytic, oxidative, and photolytic degradation products. It was also linear, precise, accurate, and robust, being suitable for routine QC analyses and stability studies. The developed HPLC method was compared to a previously described spectrophotometric method.


2009 ◽  
Vol 92 (4) ◽  
pp. 1082-1088 ◽  
Author(s):  
Rashmin B Patel ◽  
Mrunali R Patel ◽  
Madhira B Shankar ◽  
Kashyap K Bhatt

Abstract This paper describes validated HPLC and HPTLC methods for simultaneous determination of alprazolam (ALP) and fluoxetine hydrochloride (FXT) in pure powder and formulation. The HPLC separation was achieved on a Nucleosil C8 column (150 mm length, 4.6 mm id, 5 m particle size) using acetonitrilephosphate buffer pH 5.5 (45 + 55, v/v) as the mobile phase at a flow rate of 1.0 mL/min at ambient temperature. The HPTLC separation was achieved on an aluminum-backed layer of silica gel 60F254 using acetonetolueneammonia (6.0 + 3.5 + 0.5, v/v/v) as the mobile phase. Quantification in the HPLC method was achieved with UV detection at 230 nm over the concentration range 414 g/mL for both drugs, with mean recovery of 99.95 0.38 and 99.85 0.56 for ALP and FXT, respectively. Quantification in the HPTLC method was achieved with UV detection at 230 nm over the concentration range of 4001400 ng/spot for both drugs, with mean recovery of 99.32 0.45 and 99.78 0.81 for ALP and FXT, respectively. These methods are simple, precise, and sensitive, and they are applicable for the simultaneous determination of ALP and FXT in pure powder and formulations.


2012 ◽  
Vol 9 (1) ◽  
pp. 340-344 ◽  
Author(s):  
V. Bhaskara Raju ◽  
A. Lakshmana Rao

An accurate and preciseHPLCmethod was developed for the determination of lisinopril. Separation of the drug was achieved on a reverse phase C8column using a mobile phase consisting of phosphate buffer and methanol in the ratio of 35:65v/v. The flow rate was 0.8 mL/min and the detection wavelength was 215 nm. The linearity was observed in the range of 20-60 μ g/mL with a correlation coefficient of 0.9992. The proposed method was validated for its linearity, accuracy, precision and robustness. This method can be employed for routine quality control analysis of lisinopril in tablet dosage forms.


2010 ◽  
Vol 7 (1) ◽  
pp. 180-184 ◽  
Author(s):  
D. Anantha Kumar ◽  
G. Srinivasa Rao ◽  
J. V. L. N. Seshagiri Rao

A simple, accurate and reproducible RP-HPLC method has been developed for the simultaneous determination of lamivudine, zidovudine and abacavir in tablet dosage forms. Chromatography was carried out on a HiQ Sil C 18 V column using a mobile phase consisting of 0.01 M potassium dihydrogenortho-phosphate (pH 3.0) and methanol (55:45 v/v) at a flow rate of 0.8 mL/min. The detection was made at 272 nm and stavudine was used as the internal standard for this study. The retention times for lamivudine, abacavir and zidovudine were found to be 3.8, 6.3, 8.1 min. respectively. The calibration curves were linear over the range 5-250 μg/mL for both zidovudine and abacavir and 5-140 μg/mL for lamivudine. The proposed method was validated as per ICH and USP guidelines and it was found suitable for the routine quality control analysis of the drugs in tablet dosage forms.


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