Development and validation of an analytical method for the determination of related substances in bisoprolol fumarate in dosage forms by HPLC-UV-DAD

Abstract An easy and simple analytical method was standardized and validated for the estimation of residues of spirotetramat and its metabolite spirotetramat cis enol in various substrates: okra fruits, brinjal leaves and fruits, green chili, red chili, and soil. The samples were extracted with acetonitrile, diluted with brine solution, partitioned into dichloromethane, dried over anhydrous sodium sulfate, and cleaned up by treatment with activated charcoal powder. Final clear extracts were concentrated under vacuum and reconstituted with HPLC grade acetonitrile. Residues were estimated using HPLC with a photodiode array detector and a C18 column, and confirmed by HPTLC. Acetonitrile was used as the mobile phase at 0.4 mL/min. Both spirotetramat and spirotetramat cis enol presented distinct peak at retention times of 8.518 and 7.598 min, respectively. Consistent recoveries ranging from 82 to 97% for spirotetramat and spirotetramat cis enol were observed when samples were spiked at 1.00 to 0.03 mg/kg levels. The LOQ of the method was found to be 0.03 mg/kg. The analytical method was validated in terms of parameters, including selectivity, linearity, precision, and accuracy.

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Development and Validation of a Green Analytical Method for the Determination of Norfloxacin in Raw Material by FTIR Spectrophotometry

Journal of AOAC International ◽

10.5740/jaoacint.16-0177 ◽

2016 ◽

Vol 99 (6) ◽

pp. 1533-1536 ◽

Cited By ~ 5

Author(s):

Jéssica Sayuri Hisano Natori ◽

Eliane Gandolpho Tótoli ◽

Hérida Regina Nunes Salgado

Keyword(s):

Urinary Tract ◽

Organic Solvents ◽

Analytical Method ◽

Environmentally Friendly ◽

Raw Material ◽

Waste Generation ◽

Ftir Spectrophotometry ◽

Tract Infections ◽

Development And Validation

Abstract Norfloxacin is a broad-spectrum antimicrobial agent, widely used in humans and animals for the treatment of urinary tract infections. It is a second-generation fluoroquinolone. Several analytical methods to analyze norfloxacin have been described in the literature. However, most of them are complex and require the use of large amounts of organic solvents. This paper describes the development and validation of a green analytical method for the determination of norfloxacin in raw material by FTIR spectrophotometry. This method does not require the use of organic solvents, minimizing waste generation in the process and its environmental impacts. The development of methods that promote the reduction, prevention, or elimination of waste generation has become highly attractive to the pharmaceutical industry because of the growing demand from civil society and government authorities for environmentally friendly products and services. The FTIR spectrophotometry method was validated according to International Conference on Harmonization guidelines, showing adequate linearity (r = 0.9936), precision, accuracy, and robustness. This validated method can be used as an environmentally friendly alternative for the quantification of norfloxacin in raw material in QC routine analysis.

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Oxcarbazepine: validation and application of an analytical method

Brazilian Journal of Pharmaceutical Sciences ◽

10.1590/s1984-82502010000200013 ◽

2010 ◽

Vol 46 (2) ◽

pp. 265-272 ◽

Cited By ~ 2

Author(s):

Paula Cristina Rezende Enéas ◽

Renata Barbosa de Oliveira ◽

Gerson Antônio Pianetti

Keyword(s):

Spectrophotometric Method ◽

Analytical Method ◽

Disintegration Time ◽

International Conference ◽

Pharmacopoeial Monograph ◽

Development And Validation ◽

Excipient Compatibility

Oxcarbazepine (OXC) is an important anticonvulsant and mood stabilizing drug. A pharmacopoeial monograph for OXC is not yet available and therefore the development and validation of a new analytical method for quantification of this drug is essential. In the present study, a UV spectrophotometric method for the determination of OXC was developed. The various parameters, such as linearity, precision, accuracy and specificity, were studied according to International Conference on Harmonization Guidelines. Batches of 150 mg OXC capsules were prepared and analyzed using the validated UV method. The formulations were also evaluated for parameters including drug-excipient compatibility, flowability, uniformity of weight, disintegration time, assay, uniformity of content and the amount of drug dissolved during the first hour.

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