Author(s): C. Hazarathaiah Yadav, A. Malli Babu

Email(s): mallibabua@gmail.com

DOI: 10.52711/0974-360X.2021.00900   

Address: C. Hazarathaiah Yadav, A. Malli Babu*
Department of Chemistry, Vel Tech Rangarajan Dr. Sagunthala R and D Institute of Science and Technology, Avadi, Chennai - 600062, India.
*Corresponding Author

Published In:   Volume - 14,      Issue - 10,     Year - 2021


ABSTRACT:
Residual solvent testing is an integral part of reference material certification. A gas chromatography/flame ionization detector/headspace method has been developed and validated to detect and quantitate commonly used residual solvents in our production processes: Methanol, Tetrahydrofuran, Toluene, Dichloromethane and Dichloroethane in Simeprevir API. A simple and selective HS-GC method is described for the determination & quantification of Residual Solvents in Simeprevir API. Chromatographic separation was achieved on USP G43 equivalent capillary column Thermo Scientific™ Trace GOLD™ TG-624 SilMS, 30m × 0.32mm × 1.8µm column (P/N 26059-3390) using nitrogen as carrier gas by using different temperature gradient of FID Detectors. Linearity was observed in the range 40-120% of standard concentrations for Methanol, Tetrahydrofuran, Toluene, Dichloromethane and Dichloroethane (r2>0.999) for the amount of solvent estimated by the proposed methods was in good agreement. The proposed methods were validated. The accuracy of the methods was assessed by recovery studies at three different levels. Recovery experiments indicated the absence of interference from commonly encountered diluent and API. The method was found to be precise as indicated by the repeatability analysis, showing %RSD less than 10 for Methanol, Tetrahydrofuran, Toluene, Dichloromethane and Dichloroethane. All statistical data proves validity of the methods and can be used for routine analysis of pharmaceutical active ingredients for estimation of Residual Solvents of Methanol, Tetrahydrofuran, Toluene, Dichloromethane and Dichloroethane in Simeprevir. Baseline separation of all five solvents and Simeprevir API is achieved within 20.5 minutes of analysis time. Method validation comprised the following parameters: limit of detection (LOD), limit of quantitation (LOQ), linearity and range, accuracy, precision (repeatability and intermediate precision), system suitability, specificity, and robustness. Linearity and LOQ (ppm) are listed for each solvent in manuscript. The present method was proven to be robust and accurate for quantitative analysis of residual solvent in neat materials.


Cite this article:
C. Hazarathaiah Yadav, A. Malli Babu. Development and Validation of Head-space Gas Chromatographic Method in Tandem with Flame ionized detection for the determination of Residual solvents in Simeprevir API Synthesis. Research Journal of Pharmacy and Technology. 2021; 14(10):5175-1. doi: 10.52711/0974-360X.2021.00900

Cite(Electronic):
C. Hazarathaiah Yadav, A. Malli Babu. Development and Validation of Head-space Gas Chromatographic Method in Tandem with Flame ionized detection for the determination of Residual solvents in Simeprevir API Synthesis. Research Journal of Pharmacy and Technology. 2021; 14(10):5175-1. doi: 10.52711/0974-360X.2021.00900   Available on: https://rjptonline.org/AbstractView.aspx?PID=2021-14-10-18


REFERENCES:
1.    G. M. Lauer and B. D. Walker, N. Engl. J. Med., 2001, 345, 41 — 52.
2.    M. W. Fried, M. L. Shiffman, K. R. Reddy, C. Smith, G. Marinos,
F. L. Gonçales Jr, D. Häussinger, M. Diago, G. Carosi and D. Dhumeaux, N. Engl. J. Med., 2002, 347, 975 —982.
3.    M. P. Manns, J. G. McHutchison, S. C. Gordon, V. K. Rustgi, M. Shiffman, R. Reindollar, Z. D. Goodman, K. Koury, M.-H. Ling and J. K. Albrecht, Lancet, 2001, 358, 958 —965.
4.    S. Ouwerkerk-Mahadevan, M. Beumont-Mauviel, S. Mortier, M. Peeters, R. Verloes, C. Truyers, G. Mannens, I. Wynant and A. Simion, Drugs R&D, 2015, 15, 261 —270.
5.    PubChem Database, Simeprevir, 2019.
6.    A. Ariaudo, F. Favata, A. De Nicolò, M. Simiele, L. Paglietti, L. Boglione, C. S. Cardellino, C. Carcieri, G. Di Perri and A. D'avolio, J. Pharm. Biomed. Anal., 2016, 125, 369 —375.
7.    I. Vanwelkenhuysen, R. De Vries, P. Timmerman and T. Verhaeghe, J. Chromatogr. B: Anal. Technol. Biomed. Life Sci., 2014, 958, 43 —47.
8.    G. Nannetti, S. Pagni, S. G. Parisi, A. Alberti, A. Loregian and G. Palù, J. Pharm. Biomed. Anal., 2016, 121, 197 —203
9.    International Conference on Harmonization (ICH) of Technical Requirements for the Registration of Pharmaceuticals for Human Use, Q3C (R4): Impurities: guideline for residual solvents, Step 4, July 1997.
10.    (2) International Conference on Harmonization, Guidance on impurities: residual solvents. Fed. Regist. 62: 67377-88, 1997.
11.    (3) USP <467>, General Chapter on Organic volatile impurities, United States Pharmacopeia, (USP 32-NF 27). Pharmacopoeia Convention Inc., Rockville, Maryland, August 2009.
12.    (4) Residual Solvents (5.4), European Pharmacopoeia, Supplement 4.6, Directorate for the Quality of Medicines of the Council of Europe, Strasbourg, fourth edition, 2004, p. 3911.
13.    (4)C. Hazarathaiah Yadav* and D. Munirajasekhar, Research, 2014, 6(7):109-116, Journal of Chemical and Pharmaceutical Development and validation of a headspace gas chromatographic method for the determination of ethyl alcohol in ketorolac tromethamine injection(5.4)
14.    Nakka Raju, P. Raveendra Reddy, P. Janaki Pathi, N. Appala Raju. Visible Spectrophotometric estimation of Simeprevir in Pharmaceutical Formulations. Research J. Pharm. and Tech 2018; 11(9): 4157-4160.
15.    J. Ramesh Babu, J. Suhasini, S. Vidyadhara. Residual Solvents in Bendamustine Hydrochloride By Headspace Chromatography. Asian J. Pharm. Ana. 2018; 8(1): 07-12.
16.    Ali Ismail, Youssef Alahmad. Determination of ethanol and n- hexane residues in bulk rosuvastatin and atorvastatin and their dosage forms using HS-GC-MS developed method. Research J.Pharm. And Tech 2018; 11(11): 4829-4836.
17.    Tentu Nageswara Rao, T.B. Patrudu, Suneel Kumar. A, N. Krishna Rao, Karri Apparao. A New Analytical Method Validation and Quantification of Residual Solvents in Telmisartan Bulk Drug Product by Headspace gas Chromatographic Method. Research J. Science and Tech. 2018; 10(2): 98-104.
18.    Prashanthi. Y, Tentu Nageswara Rao, Yellapu Srinivas. Method Development and Validation of Alectinib Drug by RP-HPLC in Bulk and Pharmaceutical Dosage Form. Asian J. Pharm. Ana. 2018; 8(4): 186-190.
19.    B. M. Rajeshwari, Rautary T. R, Patil S. J.. Measurement of Linear and Mass attenuation Coefficient Studies of Compounds in Organic Acids. Asian J. Research Chem. 2017; 10(5): 629-634.
20.    Anil G Markandeya, Narayan P Firke, Suneeti S Gore, Sunita Salunke Gawali, Shirish S Pingale. Antibacterial Activity of Celocia argentea Leaves Extract in Organic Solvents. Research Journal of Pharmacology and Pharmacodynamics. 2014; 6(2): 79- 81.
21.    Y. Phalguna, Noor Jahan, Indraja N, Satheesh Kumar G;. Analytical Method Development and Validation for the Estimation of Sacubitril and Valsartan in Combined Pharmaceutical Dosage Forms by RP-HPLC. Asian J. Res. Pharm. Sci. 2018; 8(1): 09-16.
22.    Audumbar Mali, Ankush Hake, Manoj Patil, Ritesh Bathe, Ashpak Tamboli. Simultaneous UV Spectrophotometric Methods for Estimation of Paracetamol and Domperidone in Bulk and Tablet Dosage Form. Asian J. Res. Pharm. Sci. 6(1): Jan.-Mar., 2016; Page 21-26.
23.    S. Ashutosh Kumar, Arumbaka Harish, Manidipa Debnath, N. Sai Krishna, J. Saravanan, V. Greeshma, Ch. Naga Madhusudhan Rao. A New, Simple and Accurate Method Development and Validation for Simultaneous Estimation of Esomeprazole and Itopride in Pharmaceutical Dosage Form by Using RP –HPLC. Research J. Pharm. and Tech. 7(2): Feb. 2014; Page221-228.
24.    Simeprevir A macrocyclic hcv protease inhibitorTalwani, R., Heil, E.L., Gilliam, B.L., Temesgen, Z. Drugs of Today Volume 49, Issue 12, December 2013, Pages 769-779.

Recomonded Articles:

Author(s): Ravindranath S. Misal, Vishawas R. Potphode, Vijay R. Mahajan

DOI: 10.5958/0974-360X.2017.00218.9         Access: Open Access Read More

Author(s): Niharika, Navneet Verma

DOI: 10.5958/0974-360X.2016.00182.7         Access: Open Access Read More

Author(s): A. S. K. Sankar, B. Datchayani, N. Balakumaran, Mohammed Rilwan, R. Subaranjani

DOI: 10.5958/0974-360X.2017.00047.6         Access: Open Access Read More

Author(s): Peethala Prathyusha, Raja Sundararajan, Palyam Bhanu, Mathrusri Annapurna Mukthinuthalapati

DOI: 10.5958/0974-360X.2020.00507.7         Access: Open Access Read More

Author(s): Vijayalakshmi. S , Disalva. X, Chittaranjan Srivastava, Arun A

DOI: 10.5958/0974-360X.2019.00520.1         Access: Open Access Read More

Author(s): Yarnykh T. G., Kotvitska A. A., Tykhonov A. I., Rukhmakova O. A.

DOI: 10.5958/0974-360X.2020.00614.9         Access: Open Access Read More

Author(s): R. P. Bhole, S. R. Jagtap, K. B. Chadar, Y. B. Zambare

DOI: 10.5958/0974-360X.2020.00189.4         Access: Open Access Read More

Author(s): Suha Alnaeb, Youssef Alahmad, Saleh Trefi

DOI: 10.5958/0974-360X.2019.01035.7         Access: Open Access Read More

Author(s): Dhara Parekh, Pankaj Kapupara, Ketan Shah

DOI: dharaparekh92@gmail.com         Access: Open Access Read More

Author(s): R Deveswaran, S Bharath, BV Basavaraj, Sindhu Abraham, Sharon Furtado, V Madhavan

DOI:         Access: Open Access Read More

Author(s): Rekha Rajendran, R Hemachander, T Ezhilarasan, C Keerthana, DL Saroja, KV Saichand, Mohamed Gasim Abdullah

DOI: Not Available         Access: Open Access Read More

Author(s): Bahubali N. Patil, Vamshi Krishna Tippavajhala, Girish Pai K

DOI: 10.5958/0974-360X.2019.00140.9         Access: Open Access Read More

Author(s): Mythili. L, GNK. Ganesh, C. Monisha, Kayalvizhi. R

DOI: 10.5958/0974-360X.2019.00426.8         Access: Open Access Read More

Author(s): U.S Mahadeva Rao, Khamsah Suryati Mohd, Abdurrazaq Muhammad, Bashir Ado Ahmad, Mohaslinda Mohamad, Rosmawati Mat Ali

DOI: Not Available         Access: Open Access Read More

Author(s): Prabhakar Panzade, Prashant K Puranik

DOI: Not Available         Access: Open Access Read More

Research Journal of Pharmacy and Technology (RJPT) is an international, peer-reviewed, multidisciplinary journal.... Read more >>>

RNI: CHHENG00387/33/1/2008-TC                     
DOI: 10.5958/0974-360X 

0.38
2018CiteScore
 
56th percentile
Powered by  Scopus


SCImago Journal & Country Rank


Recent Articles




Tags