Characterization and relative response factor determination of process related impurity in Naproxen by nuclear magnetic resonance spectroscopy

Iqbal, Md. Yakub; Rao, Kollipara Mohan; Sridhar, G.; Raju, P. Padmanabha; Deshpande, Girish R.; Babu, J. Moses

doi:10.1016/j.jpba.2011.06.003

Cited by 18 publications

(5 citation statements)

References 14 publications

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“…In view of the advantages and disadvantages of chromatography and 1 H-qNMR listed above, the combination of 1 H-qNMR and chromatography has been investigated. − In the previous work, NMR was used as a nonspecific detector to determine RRF with one reference standard different from analytes. The online LC-NMR system is effective for this purpose, − however high running costs related to the use of deuterated solvents as mobile phase prevents its popularization.…”

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confidence: 99%

“…On the other hand, offline NMR was also applied to determine organic compounds separated by LC without their own reference standards. , We have applied this method for natural product analyses, quantification of quassin and neoquassin in Jamaica Quassia extracts . For this method, a reference standard is used as an internal standard for both 1 H-qNMR and chromatography to estimate the relative molar sensitivity ( RMS ) for each analyte.…”

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confidence: 99%

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Determination of PAHs in Solution with a Single Reference Standard by a Combination of ¹H Quantitative NMR Spectroscopy and Chromatography

et al. 2017

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We have applied a combination of H quantitative NMR spectroscopy (H-qNMR) and chromatography (GC or LC) to establish reliable analytical methods (qNMR/GC and qNMR/LC) for organic compounds. In this method, a reference standard is used as an internal standard for both H-qNMR and chromatography to estimate relative molar sensitivity (RMS) for analytes. The RMS values are calculated from the molar ratios between analytes and the reference standard obtained byH-qNMR; and the response ratio between them obtained by chromatography. Concentrations of analytes in the organic solution can be simultaneously determined from the RMS and amount of the reference standard added in the sample solution. This analytical method is an innovative one because only one reference standard with International System of Units (SI)-traceable property value, purity, or concentration, is necessary to determine accurate concentrations of multiple organic components in organic solutions, without the respective certified reference standards for various analytes. To verify this method, a certified reference material, NIST SRM 1647f, was used. Among the 16 polycyclic aromatic hydrocarbons (PAHs) included in NIST SRM 1647f, naphthalene and benzo[a]pyrene were selected as analytes for this method, using 1,4-bis(trimethylsilyl)benzene-d as the reference standard. Each quantitative value obtained by qNMR/GC and qNMR/LC agreed with each certified value within its expanded uncertainty.

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Determination of PAHs in Solution with a Single Reference Standard by a Combination of ¹H Quantitative NMR Spectroscopy and Chromatography

et al. 2017

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“…A relatively new 'qNMR/chromatography' technique does not mean a physical connection of an NMR spectrometer and a chromatograph. The concept was proposed in 2009 [57,58]. In the cases of quantification by internal standard methods with chromatographs, ratios between responses of the analyte and the internal standard (IS), and those between amount (i.e.…”

Section: Qnmr/chromatographymentioning

confidence: 99%

Conventional and new traceability schemes of organic standards for safe water supply in Japan

et al. 2019

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Metrological traceability to the International System of Units (SI) is required to ensure reliability of analytical results. For this purpose, SI-traceable standard solutions of respective analytes are essential for common analytical methods such as chromatography. However, it is not so easy to fulfill demands due to the existence of a vast number of targets, especially in the case of organic analysis. Because high-purity organic materials which are raw materials of standard solutions must be characterized by compound-independent methods, the mass balance approach (subtraction method) and the primary methods of measurement (e.g. the freezing point depression method and titrimetry) are used. Recently, quantitative NMR (qNMR) has been popularized.

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“…Several analytical methods have been reported in the literature for individual determination of sumatriptan and its related substances and naproxen and its related substances . Other methods are also reported for simultaneous estimation of both active pharmaceutical ingredients (APIs) by HPLC and UV spectrophotometry .…”

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confidence: 99%

Quality-by-design-based ultra high performance liquid chromatography related substances method development by establishing the proficient design space for sumatriptan and naproxen combination

et al. 2015

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Quality-by-design-based methods hold greater level of confidence for variations and greater success in method transfer. A quality-by-design-based ultra high performance liquid chromatography method was developed for the simultaneous assay of sumatriptan and naproxen along with their related substances. The first screening was performed by fractional factorial design comprising 44 experiments for reversed-phase stationary phases, pH, and organic modifiers. The results of screening design experiments suggested phenyl hexyl column and acetonitrile were the best combination. The method was further optimized for flow rate, temperature, and gradient time by experimental design of 20 experiments and the knowledge space was generated for effect of variable on response (number of peaks ≥ 1.50 - resolution). Proficient design space was generated from knowledge space by applying Monte Carlo simulation to successfully integrate quantitative robustness metrics during optimization stage itself. The final method provided the robust performance which was verified and validated. Final conditions comprised Waters® Acquity phenyl hexyl column with gradient elution using ammonium acetate (pH 4.12, 0.02 M) buffer and acetonitrile at 0.355 mL/min flow rate and 30°C. The developed method separates all 13 analytes within a 15 min run time with fewer experiments compared to the traditional quality-by-testing approach.

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Characterization and relative response factor determination of process related impurity in Naproxen by nuclear magnetic resonance spectroscopy

Cited by 18 publications

References 14 publications

Determination of PAHs in Solution with a Single Reference Standard by a Combination of ¹H Quantitative NMR Spectroscopy and Chromatography

Determination of PAHs in Solution with a Single Reference Standard by a Combination of ¹H Quantitative NMR Spectroscopy and Chromatography

Conventional and new traceability schemes of organic standards for safe water supply in Japan

Quality-by-design-based ultra high performance liquid chromatography related substances method development by establishing the proficient design space for sumatriptan and naproxen combination

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Characterization and relative response factor determination of process related impurity in Naproxen by nuclear magnetic resonance spectroscopy

Cited by 18 publications

References 14 publications

Determination of PAHs in Solution with a Single Reference Standard by a Combination of 1H Quantitative NMR Spectroscopy and Chromatography

Determination of PAHs in Solution with a Single Reference Standard by a Combination of 1H Quantitative NMR Spectroscopy and Chromatography

Conventional and new traceability schemes of organic standards for safe water supply in Japan

Quality-by-design-based ultra high performance liquid chromatography related substances method development by establishing the proficient design space for sumatriptan and naproxen combination

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Determination of PAHs in Solution with a Single Reference Standard by a Combination of ¹H Quantitative NMR Spectroscopy and Chromatography

Determination of PAHs in Solution with a Single Reference Standard by a Combination of ¹H Quantitative NMR Spectroscopy and Chromatography