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Volume: 9, Issue: 5, May, 2019
A novel analytical liquid chromatography-tandem mass spectrometry method for the estimation of Gemfibrozil in bulk and pharmaceutical formulationsAuthor Affiliations
The current study reports on a mass spectrometric method for the quantification of gemfibrozil drug substance in its formulation. Isocratic method was used for separation with help of Zorbax SB C18 column (4.6 × 50 mm, 3 μm) using a triple quadrupole mass detector in multiple reaction monitoring (MRM) mode and electrospray ionization as ionization source. The resulting runtime was found to be 3 minutes and the analyte elutes at 1.201 minutes 10-mM ammonium formate was adjusted to pH 3.5: methanol (20:80 V/V) was used as mobile phase. Increased sensitivity from selective ion monitoring (SIM) to MRM resulted in decreased quantitation limit (LOQ) and 0.5 ng/ml as detection limit (LOD). The method was validated in a range of 1–50 ng/ml and a correlation coefficient of 0.999. The method recovery was found to be in the range of 94.03 % to 100.02 %. The developed method was validated as per the International Conference on Harmonisation (ICH) guidelines.
Copyright: The Author(s). This is an open access article distributed under the Creative Commons Attribution Non-Commercial License, which permits unrestricted use, distribution, and reproduction in any medium, provided the original work is properly cited.
Drug information. [Online]. Available via http://www.drugs.com (Accessed 10 October 2018).
Gonza'lez-Pen˜as E, Agarraberes S, Ocariz AL, Quetglas EG, Campanero MA, Carballal JJ, Honorato J. A sensitive method for the determination of gemfibrozil in human plasma samples by RP-LC. J Pharm Biomed Anal, 2001; 26:7-14. https://doi.org/10.1016/S0731-7085(01)00369-7
ICH. Q3B validation of analytical procedures: methodology, International Conference on Harmonization. November 1996 [Online]. Available via https://www.fda.gov/downloads/drugs/guidances/ ucm073384.pdf (Accessed 20 October 2018).
Kang X, Wang F, Xie Z, Li H. A high performance liquid chromatography method for simultaneous determination of rosiglitazone and gemfibrozil in human plasma. J Chromatogr B, 2009; 877(7):645-8. https://doi.org/10.1016/j.jchromb.2009.01.001
Kim CK, Jae JP, Hwang HR, Ban E, Maeng JE, Kim MK, Piao XL. Simple and sensitive HPLC method for determination of gemfibrozil in human plasma with fluorescence detection. J Liq Chromatogr Rel Tech, 2006; 29(3):403-14. https://doi.org/10.1080/10826070500452051
Rao KN, Satyanarayanaa PVV, Suneethaa G, Venkateswarlu P. Development and validation of sensitive RP- HPLC method for determination of gemfibrozil in human plasma. Der Pharma Chemica, 2012; 4(3):882-8.
Rower JE, Bushman LR, Hammond KP, Kadam RS, Aquilante CL. Validation of an LC/MS method for the determination of gemfibrozil in human plasma and its application to a pharmacokinetic study. Biomed Chromatogr, 2010; 24(12):1300-8. https://doi.org/10.1002/bmc.1440
Sushma A, Harinadha Babu K, Vijay Kumar G. New analytical method development and validation for the estimation of gemfibrozil in bulk and pharmaceutical formulation by RP-HPLC. Int J Pharm, 2013; 3(1):173-5.
Ulu ST. LC determination of gemfibrozil in tablets. Chromatographia, 2006; 64. https://doi.org/10.1365/s10337-006-0057-x
Vittal S, Shitut NR, Kumar TR, Vinu MC, Mullangi R, Srinivas NR. Simultaneous quantitation of rosuvastatin and gemfibrozil in human plasma by high-performance liquid chromatography and its application to a pharmacokinetic study. Biomed Chromatogr, 2006; 20(11):1252-9. https://doi.org/10.1002/bmc.692