scholarly journals Simultaneous analysis of first-line anti-tuberculosis drugs in tablets by UV spectrophotometry compared to capillary zone electrophoresis

2012 ◽  
Vol 10 (6) ◽  
pp. 1808-1816 ◽  
Author(s):  
Luiza Marcellos ◽  
Adriana Faria ◽  
Marcus Souza ◽  
Mariana Almeida ◽  
Guilherme Sabin ◽  
...  

AbstractThe development and optimization of a novel UV spectrophotometric methodology was proposed for simultaneous analysis of ethambutol (ETB), isoniazid (ISO), rifampicin (RIF) and pyrazinamide (PYR), using multivariate calibration based on the partial least squares method (PLS). The methodology was successfully applied for analysis of four-drug fixed dose combination (4-FDC) tablets used for tuberculosis treatment. A 34 Box-Behnken design, with triplicate in central point, was used for sample preparation in the calibration step. In the present case, nine latent variables were chosen for the model development that presented the smallest RMSECV and explain 98.76% of data variance in Y block (concentrations of ETB ISO, RIF and PYR) and 99.93% of data variance in X block (spectral data). PLS models for ETB, ISO, RIF and PYR presented RMSEP and R2 values of 0.23 mg L−1 and 0.971; 0.14 mg L−1 and 0.731; 0.11 mg L−1 and 0.990 and 0.57 mg L−1 and 0.972, respectively. A validation step was performed based on the comparison between the UV spectrophotometric proposed methodology and capillary zone electrophoresis (CZE) in 4-FDC real samples and no significant difference was found between two methodologies at 95% of confidence level.

2012 ◽  
Vol 7 ◽  
pp. ACI.S9940 ◽  
Author(s):  
Mohamed Salim ◽  
Nahed El-Enany ◽  
Fathallah Belal ◽  
Mohamed Walash ◽  
Gabor Patonay

A novel, quick, reliable and simple capillary zone electrophoresis CZE method was developed and validated for the simultaneous determination of sitagliptin (SG) and metformin (MF) in pharmaceutical preparations. Separation was carried out in fused silica capillary (50.0 cm total length and 43.0 cm effective length, 49 μm i.d.) by applying a potential of 15 KV (positive polarity) and a running buffer containing 60 mM phosphate buffer at pH 4.0 with UV detection at 203 nm. The samples were injected hydrodynamically for 3 s at 0.5 psi and the temperature of the capillary cartridge was kept at 25 °C. Phenformin was used as internal standard (IS). The method was suitably validated with respect to specificity, linearity, limit of detection and quantitation, accuracy, precision, and robustness. The method showed good linearity in the ranges of 10-100 μg/mL and 50-500 μg/mL with limits of detection of 0.49, 2.11 μm/mL and limits of quantification of 1.48, 6.39 μg/mL for SG and MF, respectively. The proposed method was successfully applied for the analysis of the studied drugs in their synthetic mixtures and co-formulated tablets without interfering peaks due to the excipients present in the pharmaceutical tablets. The method was further extended to the in-vitro determination of the two drugs in spiked human plasma. The estimated amounts of SG/MF were almost identical with the certified values, and their percentage relative standard deviation values (% R.S.D.) were found to be ≤1.50% (n = 3). The results were compared to a reference method reported in the literature and no significant difference was found statistically.


Holzforschung ◽  
2013 ◽  
Vol 67 (8) ◽  
pp. 887-890 ◽  
Author(s):  
Getachew Gizaw Gebremeskel ◽  
Fredrik Aldaeus

Abstract Capillary zone electrophoresis (CZE) in an alkaline glycine buffer is suggested for the quantification of lignin content in black liquors (BL). The method was first tested by an external calibration with LignoBoost lignins. Then, the lignin content in BL was determined by means of a multivariate calibration with the application of a standard normal variate filter and partial least squares approach based on five principal components. The results are in agreement with those obtained by sulfuric acid lignin precipitation combined with ultraviolet measurement of the lignin in solution. The advantage of the CZE method is its independence from the knowledge of the exact absorptivity coefficient, which is needed for direct spectrophotometric lignin determination. Moreover, interfering substances and degradation products could be recognized and excluded from lignin determination; thus, the selectivity was increased significantly.


2015 ◽  
Vol 7 (11) ◽  
pp. 4602-4607 ◽  
Author(s):  
MingHui Li ◽  
WenShen He ◽  
LiJun Zhang ◽  
ChengLi Duan

A capillary zone electrophoresis method was established for simultaneous analysis of penicillin G and penicillin acid in milk.


2018 ◽  
Vol 41 (24) ◽  
pp. 4533-4543 ◽  
Author(s):  
Lucas Mattos Duarte ◽  
Tatiane Lima Amorim ◽  
Paula Rocha Chellini ◽  
Luiz Henrique Cantarino Adriano ◽  
Marcone Augusto Leal de Oliveira

2009 ◽  
Vol 32 (6S) ◽  
pp. 7
Author(s):  
F Parente ◽  
N Ah Mew ◽  
J Jaeken ◽  
B M Gilfix

Background: The Congenital Disorders of Glycosylation (CDG) are an expanding group of metabolic diseases with a broad clinical presentation. We sought to validate a new Capillary Zone Electrophoresis (CZE) method (Sebia CAPILLARYS™ CDT) to screen for CDG. Methods: We analyzed 119 serum samples from children of varying ages and of both sexes to establish a reference range of transferrin glycoforms including CDT (Carbohydrate Deficient Transferrin). We then studied serums from 8 known CDG patients and compared the CZE results to the isoelectric focusing (IEF) profiles. We also analyzed serums after extraction from spotted Guthrie cards. Results: The mean (SD) percentage of transferrin glycoforms is 18.5 (4.4), 78.5 (4.2), 2.5 (1.3) and 0.6 (0.3) for penta-, tetra-, trisialotransferrin and CDT, respectively. There is no statistically significant difference between the different age groups analyzed (0-5, 6-11, 12-15, 16-18, and > 18 years) or between sexes. We observed a good correlation between the CZE and IEF profiles with both fresh serum and serum extracted from Guthrie cards. Conclusions: The Sebia CAPILLARYS™ CDT system is a simple and reliable method to screen for CDG in pediatric and adult patients with an unexplained clinical syndrome, particularly when the nervous system is involved.


2013 ◽  
Vol 11 (8) ◽  
pp. 1286-1296 ◽  
Author(s):  
Renata Jesus Coelho Castro ◽  
Fausto Sobrinho ◽  
Marco Sundfeld da Gama ◽  
Patrícia Castro Barra ◽  
Rosemar Antoniassi ◽  
...  

AbstractAn alternative method for extraction optimization of C18:2 n-6 and C18:3 n-3, the main precursors for the synthesis of conjugated linoleic acid (CLA), in Brachiaria ruzizienses forages was proposed. Three methods of lipid extraction were tested: 1. Hara & Radin, 2. Micro Folch and 3. Bligh & Dyer. The preliminary test showed the Hara & Radin method as the most promising procedure. Then, a 33 Box Behnken design with triplicate in the central point was applied in Hara & Radin method in order to optimize the extraction procedure. The optimization extraction was monitored by quantification of C18:2 n-6 and C18:3 n-3 through capillary zone electrophoresis (CZE). The results obtained by CZE were compared to gas chromatography (AOCS official method) in real samples using the paired t-test. No significant difference between methods was found within a 95% confidence interval (p-value= 0.937). The alternative CZE method for Brachiaria ruzizienses forages analysis has some advantages in comparison with official GC method such as, short analysis time (10 min), no derivatization step for sample preparation, absence of specific separation columns, lower analytical cost and high throughput.


2019 ◽  
Vol 102 (2) ◽  
pp. 473-479 ◽  
Author(s):  
Marwa A A Ragab ◽  
Mohamed H Abdel-Hay ◽  
Hytham M Ahmed ◽  
Sara M Mohyeldin

Abstract Background: A validated method based on capillary zone electrophoresis coupled with a diode array detector (CZE-DAD) was investigatedfor analyzing binary mixture of ibuprofen (IBU) andphenylephrine (PHE) in their bulk and combined dosage form. Objective: This binary mixture is a challenging one as IBU is acidic and PHEis alkaline, which may affect their simultaneous analysis using CZE. The literature lacks any CZE report for IBU and PHE simultaneous analysis. Methods: Fused silica capillary (85 cm × 75 μm id) was used, and the electrolyte was a 50 mM borate buffer adjusted to pH 11 with 0.5 M NaOH. Results: The concentration ranges were 5–200 and 5–100 μg/mL for IBU and PHE, respectively, using CZE. High efficiency was achieved (N > 92990). Reasonable migration time (tm) was attained (tm< 8.5 min). Conclusions: Although the results obtained by the proposed CZE method and reported HPLC method were statistically comparable, the proposed method showed lower linearity ranges, higher efficiency, and a more reasonable run time. Highlights: CZE-DAD was used for the analysis of IBU and PHE in bulk and tablets, as no report was foundfor their determination using CZE. Binary mixture is challenging due to differences in chemical and physical properties. A detailed discussion of electrophoretic parameters optimization is included. Confirmation of peak purity was attained using DAD.


2017 ◽  
Vol 63 (2) ◽  
pp. 80-86 ◽  
Author(s):  
Aura Rusu ◽  
Maria-Alexandra Sbanca ◽  
Nicoleta Todoran ◽  
Camil-Eugen Vari

Abstract Objective: Letrozole is a highly potent oral nonsteroidal aromatase inhibitor triazole derivative. The aim of this study was to quantify letrozole from bulk, pharmaceutical formulation, and spiked urine samples by developing a simple, rapid and cost effective capillary electrophoresis method. Methods: A capillary zone electrophoresis method was optimized and validated. Additionally, an UV spectrophotometry method was used for comparing results. Results:The capillary zone electrophoresis method using a 90 mM sodium tetraborate background electrolyte proved to be an efficient method for determination of letrozole in a very short time, less than 2 minutes, using 20 kV voltage, 50 mbar/2 seconds pressure and 50°C temperature as optimum parameters. Additionally, the UV spectrophotometry method proved to be simple and efficient to quantify letrozole from bulk material and pharmaceutical formulation with linearity of response between 5 to 20 μg·mL-1 concentrations. For both methods, validation parameters, including linearity, detection and quantification limits were determined. Also we proved that our electrophoretic method has potential in analyzing letrozole from biological samples, obtaining encouraging results on estimation of letrozole from spiked urine samples without any special treatment. Conclusions: To quantify letrozole from bulk material, pharmaceutical preparations, and spiked urine samples the capillary zone electrophoresis method using a tetraborate sodium background electrolyte has proven to be simple and appropriate. Also a simple UV spectrophotometric method has been developed and validated for the same purposes.


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