Quantitative determination of azathioprine in tablets by 1H NMR spectroscopy

Göǧer, Nilgün Günden; Parlatan, H K; Basan, Hasan; Berkkan, Aysel; Özden, Tuncel

doi:10.1016/s0731-7085(99)00156-9

Cited by 38 publications

(11 citation statements)

References 7 publications

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“…Though it has a lower sensitivity relative to HPLC and mass spectrometry (MS) [ 3 ], the quantitative NMR (qNMR) method possesses distinctive advantages: (1) it can be conducted without analyte reference materials; (2) it can provide structural information and does not destroy the samples; (3) it can undertake multicomponent analysis in a mixture without pre-isolation; and (4) it requires a comparatively short time [ 4 , 5 , 6 , 7 , 8 , 9 ]. Nowadays, qNMR is mainly applied to identify and quantify drugs, biological metabolites, and natural products [ 10 , 11 , 12 , 13 , 14 , 15 , 16 ]. The basis of qNMR is the proportional relationship between the given integral resonance and the number of protons.…”

Section: Introductionmentioning

confidence: 99%

The Application of Quantitative 1H-NMR for the Determination of Orlistat in Tablets

et al. 2017

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A quantitative nuclear magnetic resonance (qNMR) method to measure the content of Orlistat in tablets was studied and found to be efficient, accurate, reliable, and simple. In this paper, phloroglucinolanhydrous and dimethylsulfoxide-d6 (DMSO-d6) served as the internal standard and solvent, respectively. The qNMR methodology, including the linearity, range, the limit of detection (LOD) and quantification (LOQ), stability, precision, and accuracy, was validated seriatim, and the results were very favorable. The content determination results of three batches of Orlistat in tablets were almost identical upon comparing the qNMR method and the high-performance liquid chromatography (HPLC) method. The recommended method authentically compensated the deficiencies of the current HPLC method for determining Orlistat content, and proved to be a method complementary to traditional analysis for the purity measurement of Orlistat in some pharmaceutical preparations.

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Section: Introductionmentioning

confidence: 99%

The Application of Quantitative 1H-NMR for the Determination of Orlistat in Tablets

et al. 2017

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“…Although the sensitivity of qNMR method is lower than chromatographic methods, qNMR method has some advantages over chromatographic methods [7]. In order to create calibration graph, qNMR method does not need a pure reference material [8], qNMR method performs structural characterization instead of destroying the sample, and analysis of mixtures can be performed without pre-isolation process using qNMR method. The basis of qNMR is relationship between integral value of signal and the proton numbers.…”

Section: Introductionmentioning

confidence: 99%

The application of qNMR for the determination of rosuvastatin in tablet form

Dıkmen¹,

Uslu²

2021

Turk J Chem

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In this study, quantative nuclear magnetic resonance (qNMR) method was used to determine the content of rosuvastatin in tablet. Linearity, range, limit of detection (LOD), limit of quantification (LOQ), accuracy and precision were determined in validation study of rosuvastatin. Furthermore, validation study of rosuvastatin was performed with high performance liquid chromatography (HPLC). Uncertainties of qNMR and HPLC methods were determined using per EURACHEM/CITAC Guide CG 4 (3th edition), Quantifying Uncertainty in Analytical Measurement. qNMR and HPLC methods were linear in the ranges of 0.10-5.00 mg/mL and 0.001-0.0995 mg/mL, respectively and these lineraties indicate very good linearity performance with regression coefficients (R2 value) above > 0.99. Moreover, LOD and LOQ values using qNMR method were observed as 0.25 mg/mL and 0.80 mg/mL, respectively. These 2 value using HPLC method were found as 0.00051 µg/mL and 0.001695 µg/mL, respectively. The strengths and weaknesses of qNMR method and HPLC method were determined with spectral emphasis on the role of identical reference standards in qualitive and quantative analyses. It was found that qNMR method is simple, efficient, reliable and accurate method. Moreover, qNMR method is an easy, practical and useful method for the validation and optimization of rosuvastatin in the tablet.

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“…Several analytical methods such as spectrophotom etry [20,21], HPLC [22,23], titrimetry [24], and H NMR [25] have been reported for the determina tion of AZT in body fluids. However, these methods suffer from some disadvantages such as high costs, long analysis times, low sensitivity and selectivity and requirement for complex and tedious sample pretreat ment.…”

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confidence: 99%

Voltammetric determination of immunosuppressive agent, azathioprine, by using a graphene-chitosan modified-glassy carbon electrode

Hatami

Jalali

2015

Russ J Electrochem

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Electrodeposition of graphene-chitosan (GR-CS) composite onto glassy carbon electrode was done via a simple one step strategy. Different methods were used for surface characterization which con firmed the presence of a nano structure of graphene sheets. The modified electrode was highly efficient in azathioprine analysis by square wave voltammetry. Reversibility of the redox couple of azathioprine was sig nificantly improved at the surface of GR-CS modified electrode compared to the bare electrode. A linear range of 1.0 × 10 -7 to 2.6 × 10 -5 M of azathioprine was obtained with a sensitivity of 5.54 A/M and a detection limit of 4.7 × 10 -8 M. The proposed sensor exhibited high reproducibility (RSD % = 5%) and repeatability (RSD % = 3.5%) and long term storage stability. The modified electrode was applied successfully to the accurate determination of azathioprine in pharmaceutical and blood serum samples.

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Quantitative determination of azathioprine in tablets by 1H NMR spectroscopy

Cited by 38 publications

References 7 publications

The Application of Quantitative 1H-NMR for the Determination of Orlistat in Tablets

The Application of Quantitative 1H-NMR for the Determination of Orlistat in Tablets

The application of qNMR for the determination of rosuvastatin in tablet form

Voltammetric determination of immunosuppressive agent, azathioprine, by using a graphene-chitosan modified-glassy carbon electrode

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