DEVELOPMENT AND VALIDATION OF A GAS CHROMATOGRAPHY-MASS SPECTROMETRY WITH SELECTED ION MONITORING METHOD FOR THE DETERMINATION OF TRACE LEVELS OF METHANE SULFONYL CHLORIDE AS AN IMPURITY IN ITRACONAZOLE ACTIVE PHARMACEUTICAL INGREDIENT

Authors

  • Mannem Durga Babu SVRM College (Nagarm),ANU (Guntur),Andhara Pradesh,India.
  • Surendrababu K
  • Kishore M

Abstract

ABSTRACT
Objective: To develop an accurate, precise, and linear gas chromatographic-mass spectrometry selective ion monitoring (SIM) method for quantitative
estimation of methane sulfonyl chloride (MSC) as an impurity in itraconazole (ICR) active pharmaceutical ingredient (API) at ppm level and validated
as per International Council of Harmonization (ICH) guidelines.
Methods: This method used in SIM mode mass selective detection was developed and validated for the trace level analysis of an impurity.
Chromatographic separation of MSC was achieved in 5.45 minutes and m/z value was 79 on SIM mode, ZB-5 ms 30 m × 0.25 mm × 0.25 µm column,
using helium carrier gas with 1.0 ml/min.
Results: The method was linear for MSC in ICR 1.90-7.5 µg/ml, respectively. The coefficient of correlation (r
) for the MSC was better than 0.999. The
limit of detection and limit of quantification (LOQ) obtained were 0.44 and 1.32 µg/ml. The method was fully validated, complying Food and Drug
Administration, ICH, and European Medicines Agency guidelines. Furthermore, verified precision, accuracy, LOQ precision, LOQ accuracy, ruggedness,
and robustness.
2
Conclusion: The methods were successfully validated to determination and quantification of MSC in ICR API. Hence, the method holds good for the
routine trace analysis of MSC in ICR and various pharmaceutical industries as well as academics.
Keywords: Methane sulfonyl chloride, Itraconazole, Gas chromatography-mass spectrometry, Method development, Method validation.

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References

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Published

01-07-2016

How to Cite

Durga Babu, M., S. K, and K. M. “DEVELOPMENT AND VALIDATION OF A GAS CHROMATOGRAPHY-MASS SPECTROMETRY WITH SELECTED ION MONITORING METHOD FOR THE DETERMINATION OF TRACE LEVELS OF METHANE SULFONYL CHLORIDE AS AN IMPURITY IN ITRACONAZOLE ACTIVE PHARMACEUTICAL INGREDIENT”. Asian Journal of Pharmaceutical and Clinical Research, vol. 9, no. 4, July 2016, pp. 403-7, https://mail.innovareacademics.in/journals/index.php/ajpcr/article/view/12823.

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