Development and Validation of Sensitive GC and GC-MS Methods for the Detection and Quantification of Alkyl Mesylates in Pharmaceutical Active Ingredients | Chapter 8 | Recent Developments in Chemistry and Biochemistry Research Vol. 6

Methyl, ethyl, isopropyl, and hexyl mesylates were determined at trace levels in various active pharmaceutical ingredients by the capillary gas chromatographic method using flame ionization and mass spectrometers as detectors because of their mutagenic, carcinogenic, and teratogenic potential health risks in the medicines consumed by humans. A wide-bore gas chromatographic capillary column, the DB-WAX column (30 m × 0.53 mm × 1.0 µ m), was used for method development and validation. The carrier gas is helium for GC and GCMS methods with an injection volume of 4 µ L. Standard and sample solutions were prepared in a non-polar solvent such as n-hexane with the help of the solid-liquid extraction technique. The detection and quantitation limits were 0.02 and 0.05 ppm for methyl, ethyl, isopropyl, and hexyl mesylates for the GC and GCMS methods were achieved at very low levels by enhancing the analyte concentration up to 1 g quantity. The method was validated as per the procedures provided by the International Council for Harmonization of Technical Requirements for Pharmaceuticals for Human Use (ICH) and the Food and Drug Administration (FDA) of the United States of America. The %RSD for methyl, ethyl, isopropyl, and hexyl mesylates were less than 2.5%. The linearity of the method was demonstrated from 0.02 ppm to 5 ppm with respect to the analyte concentration, and it afforded correlation coefficients exceeding 0.99. The recoveries of methyl mesylate, ethyl mesylate, isopropyl mesylate, and hexyl mesylate were in the range of 97.1 to 107.1%. Hence, this is a robust method for the determination of alkyl mesylates in these APIs. Also, this method has been verified by a gas chromatograph equipped with mass spectrometry (GC-MS) for the detection of alkyl mesylates.

 

Author (s) Details

N Balaji
Analytical Development Laboratory, Apicore LLC, New Jersey, USA.

 

Sayeeda Sultana
Department of Chemistry, St. Peter’s University, Avadi, Chennai, Tamil Nadu, India.

 

Please see the book here:- https://doi.org/10.9734/bpi/rdcbr/v6/2320

 

Method Development and Validation of Residual Solvents in Paroxetine by Gas Chromatography | Chapter 5 | Novel Aspects on Pharmaceutical Research Vol. 1

 The objective concerning this work is to evolve and validate a new gas chromatographic procedure for the simultaneous conclusion of acetone and isopropyl alcohol in Paroxetine. To decide the presence of acetone and isopropyl alcohol in paroxetine, a easy, accurate, and impressionable gas chromatographic method was conceived and validated. Using a flame ionisation indicator (FID) and gradient line, residual solvents were divided on ZB-1, 30 m length 0.53 mm ID, and film diameter 5 m. The injection was completed activity in split mode, with a split percentage of 10:1. Dimethyl acetamide was selected as a diluent to acquire good sensitivity along with the improvement. 1-Propanol was used as an within standard which working for area ratio system.The developed vapor chromatographic method offers symmetrical peak shape, good resolution of 2.3 min and judicious retention opportunity for the solvents acetone 9.21 min and isopropyl intoxicating 9.845 min. The limit of discovery for acetone and isopropyl alcohol was 26.72 µg/ml and 82.96 µg/ml, individually. Limit of quantitation for acetone and isopropyl alcohol was 80.96 µg/ml and 251.39 µg/ml, respectively. Precision was 0.83 and 0.63. Linearity was y = 0.0004x, R2 = 0.9988 for acetone, and y = 0.0001x+0.0021, R2 = 0.9987 for isopropyl intoxicating, and accuracy in addition to robustness is acted and acceptable results were obtained. Hence, The projected, developed procedure was demonstrated as simple, delicate, linearity, correct, and robust, So, this design can be used to determine the leftover organic solvent in Paroxetine drug substance and drug device. The study concluded that it can be secondhand for the determination of leftover solvents in Paroxetine API and also in the done dosage forms place the particular solvent used for the coating purpose in the drug companies and research workshops.

Author(s) Details:

S. K. Abdul Rahaman,
Department of Pharmaceutical Analysis, Nirmala College of Pharmacy, Atmakur, Mangalagiri, Guntur, Andhra Pradesh, India.

Padmavathi Sakinala,
Department of Pharmaceutical Analysis, Nirmala College of Pharmacy, Atmakur, Mangalagiri, Guntur, Andhra Pradesh, India.

N. Khaleel,
Department of Pharmaceutical Sciences, Acharya Nagarjuna University, Guntur, Andhra Pradesh, India.

Harekrishna Roy,
Department of Pharmaceutics, Nirmala College of Pharmacy, Atmakur, Mangalagiri, Guntur, Andhra Pradesh, India.

B. Pamula Reddy,
Department of Pharmaceutics, Nirmala College of Pharmacy, Atmakur, Mangalagiri, Guntur, Andhra Pradesh, India.

G. Sai Sree Lakshmi,
Department of Pharmaceutical Analysis, Nirmala College of Pharmacy, Atmakur, Mangalagiri, Guntur, Andhra Pradesh, India.

Please see the link here: https://stm.bookpi.org/NAPR-V1/article/view/10303