scholarly journals Development of membrane electrodes for selective determination of lisinopril in pharmaceuticals

Author(s):  
Nagaraju Rajendraprasad ◽  
Kanakapura Basavaiah

Abstract Background Lisinopril (LNP) is an angiotensin-converting enzyme inhibitor used as anti-hypertensive, cardiovascular, in anti-prophylactic and anti-diabetic nephropathy drug. Development of two new, simple, low cost, and selective membrane-based ion-selective electrodes has been proposed for the determination of LNP in pharmaceuticals. Methods The electrodes are based on poly(vinyl)chloride membrane doped with LNP-phosphotungstic acid (LNP-PTA) and LNP-phosphomolybdic acid (LNP-PMA) ion-pairs as molecular recognition materials. Results The developed LNP-PTA and LNP-PMA electrodes are applicable for the determination of LNP over the linear range of 5 × 10−5–2.4 × 10−3 mol l−1. The working pH ranges to measure potentials were 2.5 to 6.4 and 2.3 to 6.0 for LNP-PTA and LNP-PMA ISEs, respectively. The electrodes displayed the rapid Nernstian responses as revealed by the values of slopes 55.06 and 52.39 mV/decade, with limit of detection (LOD) values of 1.2 × 10−5 and 1.18 × 10−5 mol l−1 for LNP-PTA and LNP-PMA electrodes, respectively. The limits of quantitation (LOQ) values have also been calculated for both the electrodes. The developed electrodes have potential stability for up to 1 month and emerged as highly selective for the determination of LNP over other spiked ions and compounds. Conclusions The proposed electrodes have been validated and found that they are suitable for the determination of LNP in pharmaceuticals in pure form and in dosage forms. The results obtained in the analysis of LNP using proposed electrodes have been compared statistically with reference method’s results to assess the accuracy and precision. Robustness and ruggedness of the developed electrodes have also been checked and found satisfactory. The recovery studies have been performed by standard addition procedure to assess the role of excipients in tablets containing LNP and the results obtained are satisfactory.

2013 ◽  
Vol 19 (1) ◽  
pp. 121-128 ◽  
Author(s):  
Hemavathi Deepakumari ◽  
Shiramahally Mallegowda ◽  
Kanakapura Vinay ◽  
Hosakere Revanasiddappa

Two simple, sensitive and extraction-free spectrophotometric methods are described for the estimation of risperidone (RSP) in both pure and in pharmaceutical preparations. The proposed methods are based on the formation of ion-pair complex between RSP and the dyes, bromophenol blue (BPB) in method A and Phenol red (PR) in method B at room temperature to form yellow colored products which show maximum absorbance at 410 and at 400 nm in methods A and B, respectively. Beer's law was obeyed in the concentration range of 0.5-10 and 0.5-25 ?g mL-1 in methods A and B with apparent molar absorptivities of 3.43 ? 104 and 0.85 ? 104 L moL-1 cm-1, respectively. The limit of detection for method A is found to be 0.0056 and for method B is 0.132 ?g mL-1. The composition of the ion-pairs was established by Job?s method and it was found to be 1:1 for both the methods A and B. The proposed methods have been applied successfully to the determination of RSP in pharmaceutical preparations. The results were statistically compared with those of a reference method by applying the Student?s t-test and F-test. The methods developed were validated for accuracy and precision by performing recovery experiments via standard addition technique.


2010 ◽  
Vol 75 (5) ◽  
pp. 563-575 ◽  
Author(s):  
Moslem Mohammadi ◽  
Mehdi Khodadadian ◽  
Mohammad K. Rofouei

A plasticized poly(vinyl chloride) membrane electrode based on 4-[(5-mercapto-1,3,4-thiadiazol-2-ylimino)methyl]benzene-1,3-diol (L) for highly selective determination of palladium(II) (in PdCl42– form) is developed. The electrode showed a good Nernstian response (29.6 ± 0.4 mV per decade) over a wide concentration range (3.1 × 10–7 to 1.0 × 10–2 mol l–1). The limit of detection was 1.5 × 10–7 mol l–1. The electrode has a response time of about 20 s, and it can be used for at least 2 months without observing any considerable deviation from Nernstian response. The proposed electrode could be used in the pH range of 2.5–5.5. The practical utility of the electrode has been demonstrated by its use for the estimation of palladium content in aqueous samples.


2016 ◽  
Vol 13 (4) ◽  
pp. 829-837
Author(s):  
Baghdad Science Journal

PVC membrane sensor for the selective determination of Mefenamic acid (MFA) was constructed. The sensor is based on ion association of MFA with Dodecaphospho molybdic acid (PMA) and Dodeca–Tungstophosphoric acid(PTA) as ion pairs. Nitro benzene (NB) and di-butyl phthalate (DBPH) were used as plasticizing agents in PVC matrix membranes. The specification of sensor based on PMA showed a linear response of a concentration range 1.0 × 10–2 –1.0 × 10–5 M, Nernstian slopes of 17.1-18.86 mV/ decade, detection limit of 7 × 10-5 -9.5 × 10 -7M, pH range 3 – 8 , with correlation coefficients lying between 0.9992 and 0.9976, respectively. By using the ionphore based on PTA gives a concentration range of 1.0 × 10–4 –1.0 × 10–5 M, Nernstian slope of 17.18-18.4 mV/ decade, limit of detection 8.0 × 10–6-9.3 × 10-5M,pH range 3 – 8 and correlation coefficients range between 0.9984 and 0.9891, respectively. The measurement interferences in the presence of Li+, Na+, Mg2+ Ca2+, Fe3+and Al3+ were studied using separate and match potential methods for selectivity coefficient determination. The method was applied for the determination of Mefenamic Acid in pharmaceutical preparations


2009 ◽  
Vol 6 (s1) ◽  
pp. S163-S170 ◽  
Author(s):  
R. Singh Gujral ◽  
S. Manirul Haque ◽  
P. Shanker

An accurate and validated spectrophotometric method was developed for the determination of gabapentin. This is simple, sensitive and low cost UV spectrophotometric method. The method is based on the direct measurement of the native absorbance of the drug. The detection was done at 210 nm. The method was linear in the range of 0.25 - 3.5 µ g/mL with correlation coefficient of 0.9999. It is validated according to the ICH guidelines with respect to linearity, selectivity, accuracy and precision, limit of quantitation and limit of detection. The method has been applied to assess gabapentin in pharmaceutical formulations with good accuracy and precision and relatively free of interference from coexisting substances.


Materials ◽  
2020 ◽  
Vol 13 (10) ◽  
pp. 2275 ◽  
Author(s):  
Baraa Al-Hashimi ◽  
Heshu Sulaiman Rahman ◽  
Khalid Mohammad Omer

The determination of rifampicin in pharmaceutical dosage forms using a rapid, sensitive, selective, biocompatible, and low-cost method is of vital importance in the pharmaceutical analysis field to ensure its concentration is within the effective range when administered. In this study, nitrogen-and-phosphorous-doped carbon nanodots (CNDs) were prepared using a single-step hydrothermal method with ciprofloxacin as the starting material. The CNDs showed a highly intense blue fluorescence emission centered at 450 nm, with a photoluminescence quantum yield of about 51%. Since the absorption of rifampicin was the same as the excitation spectrum of CNDs, inner filter effect (IFE) quenching occurred and it was used as a successful detection platform for the analysis of rifampicin in capsules. The detection platform showed a dynamic linear range from 1 to 100 μM (R2 = 0.9940) and the limit of detection was 0.06 μM (when S/N = 3). The average spike recovery percentage for rifampicin in the capsule samples was 100.53% (n = 5). Moreover, the sub-chronic cytotoxicity of CNDs was evaluated on healthy male mice (Balb/c) drenched with different amounts of CNDs (10 and 50 mg/kg). During this study period, no mortalities or toxicity signs were recorded in any of the experimental subjects. Based on the cytotoxicity experiment, the proposed nano-probe is considered safe and biocompatible.


Sensors ◽  
2021 ◽  
Vol 21 (6) ◽  
pp. 1975
Author(s):  
Isabel Seguro ◽  
João G. Pacheco ◽  
Cristina Delerue-Matos

In this work, a disposable electrochemical (voltammetric) molecularly imprinted polymer (MIP) sensor for the selective determination of diclofenac (DCF) was constructed. The proposed MIP-sensor permits fast (30 min) analysis, is cheap, easy to prepare and has the potential to be integrated with portable devices. Due to its simplicity and efficiency, surface imprinting by electropolymerization was used to prepare a MIP on a screen-printed carbon electrode (SPCE). MIP preparation was achieved by cyclic voltammetry (CV), using dopamine (DA) as a monomer in the presence of DCF. The differential pulse voltammetry (DPV) detection of DCF at MIP/SPCE and non-imprinted control sensors (NIP) showed an imprinting factor of 2.5. Several experimental preparation parameters were studied and optimized. CV and electrochemical impedance spectroscopy (EIS) experiments were performed to evaluate the electrode surface modifications. The MIP sensor showed adequate selectivity (in comparison with other drug molecules), intra-day repeatability of 7.5%, inter-day repeatability of 11.5%, a linear range between 0.1 and 10 μM (r2 = 0.9963) and a limit of detection (LOD) and quantification (LOQ) of 70 and 200 nM, respectively. Its applicability was successfully demonstrated by the determination of DCF in spiked water samples (river and tap water).


2007 ◽  
Vol 4 (2) ◽  
pp. 173-179 ◽  
Author(s):  
K. Basavaiah ◽  
U. R. Anil Kumar

A simple spectrophotometric method is proposed for the determination of zidovudine(ZDV) in bulk drug and in pharmaceutical preparations. The method is based on the oxidation of ZDV by a known excess of oxidant N-bromosuccinimide (NBS), in buffer medium of pH 1.5, followed by the estimation of unreacted amount of oxidant with metol and sulphanilic acid. The reacted oxidant corresponds to the amount ZDV. The purple-red reaction product absorbs maximally at 530 nm and Beer’s law is obeyed over a range 5 to 75 μg mL-1. The apparent molar absorptivity is calculated to be 5.1×103L mol-1cm-1, and the corresponding Sandell sensitivity value is 0.052 μg cm-2. The limit of detection and quantification are found to be 0.90 and 2.72, respectively. Intra-day and inter-day precision and accuracy of the developed methods were evaluated as per the current ICH guidelines. The method was successfully applied to the assay of ZDV in tablet/capsule preparations and the results were statistically compared with those of the reference method by applying the Student’s t-test and F-test. No interference was observed from the common tablet/capsule excipients. The accuracy of the method was further ascertained by performing recovery studies via standard-addition method.


2010 ◽  
Vol 7 (3) ◽  
pp. 807-812 ◽  
Author(s):  
Vanita Somasekhar ◽  
D. Gowri Sankar

A reverse phase HPLC method is described for the determination of esmolol hydrochloride in bulk and injections. Chromatography was carried on a C18column using a mixture of acetonitrile, 0.05 M sodium acetate buffer and glacial acetic acid (35:65:3 v/v/v) as the mobile phase at a flow rate of 1 mL/min with detection at 275 nm. The retention time of the drug was 4.76 min. The detector response was linear in the concentration of 1-50 μg/mL. The limit of detection and limit of quantification was 0.614 and 1.86 μg/mL respectively. The method was validated by determining its sensitivity, linearity, accuracy and precision. The proposed method is simple, economical, fast, accurate and precise and hence can be applied for routine quality control of esmolol hydrochloride in bulk and injections.


2019 ◽  
Vol 31 (1) ◽  
pp. 1-9
Author(s):  
Deepak Kumar Sahu ◽  
Joyce Rai ◽  
Chhaya Bhatt ◽  
Manish K. Rai ◽  
Jyoti Goswami ◽  
...  

In modern age pesticide is used widely in agriculture. Lambda-cyhalothrin (LCT) is one of the most used pesticides which are used as a insecticide to kill pest, tricks, flies etc in agricultural field and it is also used for crop production. We have developed new method to detect LCT insecticide in agriculture field and reduce its uses. In this method we found the maximum absorbance at 460 nm for yellow colour dye. We also calculated limit of detection and limit of quantification 0.001 mg kg-1 and 0.056 mg kg-1 respectively. Molar absorptivity and Sandell’s sensitivity was also calculated and obtained 1.782 ×107 mol-1 cm-1 and 9.996 ×10-6 µg cm-2 respectively. The obtained yellow colour dye obeyed Beer’s law limit range of 0.5 µg ml -1 to 16 µg ml-1 in 25 ml. This method is less time consuming, selective, simple, sensitive and low cost. Present method is successfully applied in various soil, water and vegetable samples.


2018 ◽  
Vol 33 (2) ◽  
pp. 21
Author(s):  
Kanakapura Basavaiah ◽  
Okram Zenita Devi

Two sensitive spectrophotometric methods are described for the determination of simvastatin (SMT) in bulk drug and in tablets. The methods are based on the oxidation of SMT by a measured excess of cerium (IV) in acid medium followed by determination of unreacted oxidant by two different reaction schemes. In one procedure (method A), the residual cerium (IV) is reacted with a fixed concentration of ferroin and the increase in absorbance is measured at 510 nm. The second approach (method B) involves thereduction of the unreacted cerium (IV) with a fixed quantity of iron (II), and the resulting iron (III) is complexed with thiocyanate and the absorbance measured at 470 nm. In both methods, the amount of cerium (IV) reacted corresponds to SMT concentration. The experimental conditions for both methods were optimized. In method A, the absorbance is found to increase linearly with SMT concentration (r = 0.9995) whereas in method B, the same decreased (r = -0.9943). The systems obey Beer’s law for 0.6-7.5 and 0.5-5.0 μg mL-1 for method A and method B, respectively. The calculated molar absorptivity values are 2.7 X 104 and 1.06 X 105 Lmol-1 cm-1, respectively; and the corresponding sandel sensitivity values are 0.0153 and 0.0039μg cm-2, respectively. The limit of detection (LOD) and quantification (LOQ) are reported for both methods. Intra-day and inter-day precision, and accuracy of the methods were established as per the current ICH guidelines. The methods were successfully applied to the determination of SMT in tablets and the results were statistically compared with those of the reference method by applying the Student’s t-test and F-test. No interference was observed from the common excipients added to tablets. The accuracy and validity of the methods were further ascertained by performing recovery experiments via standard addition procedure.


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