GC-FID Method Development and Validation Parameters for Analysis of Palm Oil (Elaeis guineensis Jacq.) Fatty Acids Composition

Ntsomboh-Ntsefong Godswill^{1, 2,} , Ngando-Ebongue Georges Frank¹, Maho-Yalen Josian Edson^{2, 3}, Youmbi Emmanuel^{2, 4}, Bell Joseph Martin², Ngalle-Bille Hermine², Tabi-Mbi Kingsley^{1, 2}, Likeng-Li-Ngue Benoit Constant^{1, 2} and Nsimi-Mva Armand^{2, 5}

¹Lipids Analysis Laboratory, IRAD Specialized Centre for Oil Palm Research of La Dibamba, Douala-Cameroon

²Laboratory of Genetics and Plant Improvement, University of Yaounde 1, Department of Plant Biology, Yaounde-Cameroon

³University of Yaounde 1, Higher Teachers’ Training College, Department of Biological Sciences, Yaounde-Cameroon

⁴Centre Africain de Recherche sur Bananiers et Plantains (CARBAP), Njombé-Cameroun

⁵Institute of Agricultural Research for Development (IRAD), S. W. Regional Centre, Ekona-Cameroon

Cite this paper:
Ntsomboh-Ntsefong Godswill, Ngando-Ebongue Georges Frank, Maho-Yalen Josian Edson, Youmbi Emmanuel, Bell Joseph Martin, Ngalle-Bille Hermine, Tabi-Mbi Kingsley, Likeng-Li-Ngue Benoit Constant and Nsimi-Mva Armand. GC-FID Method Development and Validation Parameters for Analysis of Palm Oil (Elaeis guineensis Jacq.) Fatty Acids Composition. Research in Plant Sciences. 2014; 2(3):53-66. doi: 10.12691/plant-2-3-2

Abstract

The variety of available techniques and analytical methods applied in laboratories calls for the need of defining the scope, range of application and quality of information obtained using each of them with reference to internationally agreed standards. Of these techniques, Gas Chromatography with Flame Ionization Detector (GC-FID) is most used in fatty acids analysis. Method development and validation is useful for GC and other analytical procedures. This paper outlines the importance of method validation and elaborates on typical validation parameters with special reference to their application in the analysis of fatty acids of palm oil. The first section presents background information on stages in analytical method processing, quantitative and qualitative analysis, GC and its use in the analysis of lipid extracts. Critical components for a method are highlighted such as sampling, sample preparation (FAME derivatization), instrument analysis conditions and method standardization. Validation characteristics like Specificity, Linearity and range, Accuracy, Precision, LOD, LOQ, Robustness, Ruggedness and System suitability are presented in the last section with a brief view on some statistical methods used in method validation. It is hoped that this review will facilitate the work of analysts and the scientific community by enhancing efficient method development and validation which matches international standards.

Keywords:
GC-FID FAME preparation method development validation characteristics fatty acids Elaeis guineensis Jacq. Gas Chromatography

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References:

[1]	Cortes J. E., Suspes A., Roa S., González C., & Castro H. E., “Total petroleum hydrocarbons by gas chromatography in Colombian waters and soils”. American Journal of Environmental Science, 8 (4): 396-402, 2012.
[2]	Izydor Apostol, Ira Krull & Drew Kelner, “Analytical Method Validation for Biopharmaceuticals”. Book chapter in: Analytical Chemistry, pp. 115-134, 2012.
[3]	Ranjit S., “HPLC method development and validation- an overview”. J. Pharm. Educ. Res., 4 (1): 26-33, 2013.
[4]	Sigma-Aldrich, “Fatty Acid / FAME Application Guide. Analysis of Foods for Nutritional Needs”, sigma-aldrich.com/fame, 24 pp., 2008.
[5]	Naga D. P.V, Putta R. K., Salahuddin Md., Shanta K. S. M., “Candesartan cilexetil analytical method development and validation studies by reverse phase HPLC technique”. International Journal of Pharmaceutical Frontier Research, 2 (3): 36-43, 2012.
[6]	Cristián A, Ferretti, Carlos R., Apesteguía, & Isabel di Cosimo J., “Development and validation of a gas chromatography method for the simultaneous determination of multicomponents during monoglyceride synthesis by glycerolysis of methyl oleate: application to homogeneous and heterogeneous catalysis”. The Journal of the Argentine Chemical Society, 98: 16-28, 2011.
[7]	Martin A. J. P. and Synge R. L. M., “A new form of chromatogram employing two liquid phases”. Biochem. J. 35: 1358-0, 1941.
[8]	Ettre L. S., “Milestones in. Chromatography. The Birth of Partition Chromatography” LCGC, 19: 506-512, 2001.
[9]	Christie W. W., “Preparation of ester derivatives of fatty acids for chromatographic analysis”. In: Advances in Lipid Methodology – Two, pp. 69-111. William.W. Christie (Ed.), Oily Press, Dundee. The Scottish Crop Research Institute, Invergowrie, Dundee, Scotland DD2 5DA, 1993.
[10]	Christie,W.W., “Gas Chromatography and Lipids”, Oily Press, Ayr., 1989.
[11]	Papazova D. & Pavlova A., “Development of a Simple Gas Chromatographic Method for Differentiation of Spilled Oils”. Journal of Chromatographic Science, 37: 1-4, 1999.
[12]	Takuro W., Kenji K., Nobuhiro M., & Tsuneaki M., “Development of a Precise Method for the Quantitative Analysis of Hydrocarbons Using Post−Column Reaction Capillary Gas Chromatography with Flame Ionization Detection”. Chromatography, 27 (2): 49-55, 2006.
[13]	Lindholm J., Development and validation of HPLC methods for analytical and preparative purposes. In: Comprehensive summaries of Uppsala dissertations from the Faculty of Science and Technology 995. Acta Universitatis Upsaliensis, Uppsala, 87 pp., 2004.
[14]	Diana D., Cornella M., Vasile A., & Elena B., “Validation of a GC/HS method for ethanol quantitative analysis using as internal standard tert-butanol”. Farmacia, 59 (5): 721-727, 2011.
[15]	Imeh J. O., “Development of methods for the analysis of petroleum contaminated soils”. PhD thesis, Faculty of Engineering and Physical Sciences, School of chemical engineering and analytical science, University of Manchester, 244 pp., 2010.
[16]	AOCS, 2005. “Fatty Acid Composition by Gas Chromatography” AOCS Method Ce 1-62, AOCS Official Methods (2005) American Oil Chemists Society.
[17]	Method 8015B, “Nonhalogenated organics using GC/FID”. Revision 2, December 1996, 28p.
[18]	Svetlana H. & Eva M., “Fast Gas Chromatography and its use in pesticide residues analysis,” Book Chapter. In: Pesticides - Strategies for Pesticides Analysis, Prof. Margarita Stoytcheva (Ed.), pp. 131-155, 2011. InTech, Available from: http://www.intechopen.com/books/pesticides-strategies-for-pesticidesanalysis/fast-gas-chromatography-and-its-use-in-pesticide-residues-analysis.
[19]	AFNOR, 1988. Recueil des normes françaises sur les corps gras, graines oléagineuses, produits dérivés, 4e édition. Association française de normalisation; Paris.
[20]	Furniss B. S., Hannaford A. J., Smith P. W. G. & Tatchell A. R. (Editors), Vogel's Textbook of Practical Organic Chemistry (5th Edition), Longman Scientific & Technical, Harlow. 1989.
[21]	Indupriya M., Chandan R. S., Gurupadayya B. M., & Sowjanya K., “Quantitative determination of levetiracetam by gas chromatography using ethyl chloroformate as a derivatizing reagent in pure and pharmaceutical preparation”. International Journal of Pharmacy & Technology, 3 (1): 1694-1701, 2011.
[22]	Chowdhury K. Banu, L. A., Khan S. and Latif A., “Studies on the Fatty Acid Composition of Edible Oil”. Bangladesh J. Sci. Ind. Res. 42 (3), 311-316, 2007.
[23]	Kikta E. J. jr. & Stange A. E., “Phenones : a family of compounds broadly applicable to use as internal standards in high performance liquid chromatography.” J. Chromatogr. A, 138, 41, 1977.
[24]	Pedersen-Bjergaard S., Rasmussen K. E., Halvorsen T. G., “Liquid-liquid extraction procedures for sample enrichment in capillary zone electrophoresis.” J Chromatogr A., 902 (1): 91-105, 2000
[25]	Mohd M. S., Zalilah N., Susie L. L., Wan A. W. I., & Ahmedy A. N., “Linearity assessment according to IUPAC guidelines for the determination of plasticizers in plastic food packaging by gas chromatography”. Retrieved online on 23/4/2014. Universiti Teknologi Malaysia, 81310 Skudai, Johor, Malaysia. 21 p., 2014.
[26]	Molnar-Perl I. & Pinter-Szakacs M., “Modification in the chemical derivatization of carboxylic acids for their gas chromatography analysis.” J. Chromatogr. A, 365, 171-182, 1986.
[27]	ESA Biosciences, Simultaneous analysis of glycerides (mono, di, and triglycerides) and free fatty acids in palm oil. Corona charged aerosol detector. Application note, 3p. (Accessed online on 6/9/2013).
[28]	ICH, 2005. Q2 (R1), “Validation of analytical procedures: text and methodology”, ICH Harmonised Tripartite Guideline. International Conference on Harmonisation of Technical Requirements for Registration of Pharmaceuticals for Human Use, Chicago, USA, 2005.
[29]	Fabíola B. C., Irinaldo D. J., Pablo Q. L. & Rui O. M., “Development and Validation of Analytical Methodology and Evaluation of the Impact of Culture Conditions and Collection Associated with the Seasonality in the Production of Essential Oil of Plectranthus amboinicus (Lour) Spreng,” Dr. Bekir Salih (Ed.), ISBN: 978-953-51-0295-3, Gas Chromatography - Biochemicals, Narcotics and Essential Oils, pp. 221-237, 2012.
[30]	Gowrisankar D., Abbulu K., Bala Souri O., & Sujana K. “Validation and Calibration of Analytical Instruments.” J Biomed Sci and Res., 2 (2): 89-99, 2010.
[31]	Pedro L. G., Ernesto B., Fabio P. G. & Jose L. V. Q., “Analytical Method Validation, Wide Spectra of Quality Control”. Dr. Isin Akyar (Ed.), InTech, 19p. Available from: http://www.intechopen.com/books/wide-spectra-of-quality-control/analytical-method-validation, 2011.
[32]	Madhukar A., Prince A., Vijay Kumar R., Sanjeeva Y., Jagadeeshwar K., Raghupratap D., “Simple and sensitive analytical method development and validation of metformin hydrochloride by RP-HPLC”. International Journal of Pharmacy and Pharmaceutical Sciences, 3 (3): 117-120, 2011.
[33]	Ouattara J. P. N., Pigeon O. & Pieter S., “Validation of a multi-residue method to determine deltamethrin and alpha-cypermethrin in mosquito nets by gas chromatography with electron capture detection (GC-μECD)”. Parasites & Vectors, 6 (77): 1-11, 2013.
[34]	Lotfi S., Ines M., Bassem J. & Abdelmanef A., “Development and Validation of a Gas Chromatographic Method for Identification and Quantification of Terpene Trilactones in Ginkgo biloba L. Extract and Pharmaceutical Preparations”. The Open Chemical and Biomedical Methods Journal, 3: 18-24, 2010.
[35]	Feride K. & Emre K., “Determination of Organochlorinated Pesticide Residues by Gas Chromatography - Mass Spectrometry after Elution in A Florisil Column”. Kafkas Univ Vet Fak Derg, 17 (1): 65-70, 2011.
[36]	Noppe H., De Wasch K., Poelmans S., Van Hoof N., Verslycke T., Janssen C.R., & De Brabander H. F., “Development and validation of an analytical method for the detection of estrogens in water”. Analytical and Bioanalytical Chemistry, 382: 91-98, 2005.
[37]	Sanjay A. J., Shashikant B. L., Navanath C. N., Saroj R. B., & Vijayavitthal T. M., “Development and Validation of Stability-Indicating GC-FID Method for the Quantitation of Memantine Hydrochloride and Its Nonchromophoric Impurities in Bulk and Pharmaceutical Dosages.” Chromatography Research International, pp. 1-10, 2012.
[38]	Sharma T., & Solanki N. S., “Statistical assurance of process validation and analytical method validation of celecoxib capsules”. International Journal of Current Pharmaceutical Research, 4 (1): 80-83, 2012.
[39]	Joanna G., Urszula H., Jan K., Malgorzata T. & Jerzy J., “Development and validation of GC-FID method for the determination of ethanol residue in marjoram ointment”. Acta Poloniae Pharmaceutica-Drug Research, 66 (6): 611-615, 2009.
[40]	Seetharaman R. & Lakshmi K. S., “Development and Validation of a Reverse Phase Ultra Performance Liquid Chromatographic Method for Simultaneous Estimation of Nebivolol and Valsartan in Pharmaceutical Capsule Formulation” J Chromatograph Separat Techniq 5: 229, 2014. doi:10.4172/2157-7064.1000229
[41]	Bilal Y. & Yucel K., “Method development and validation for the GC-FID assay of 17 β-estradiol in pharmaceutical preparation”. International Journal of Pharmaceutical Sciences Review and Research, 2 (2): 44-47, 2010
[42]	Thompson M., Ellison S. L. R., & Wood R. “Harmonized guidelines for single laboratory validation of methods of analysis (IUPAC Technical Report)”. Pure Appl. Chem., 74, 835-855, 2002.
[43]	Van Den Bogaard A., Hazen M. J., & Van Boven C. P., “Quantitative Gas Chromatographic Analysis of Volatile Fatty Acids in Spent Culture Media and Body Fluids.” Journal of Clinical Microbiology, 23 (31986): 523-530, 1986.
[44]	Katan M. B., “Trans fatty acids and plasma lipoproteins. Overview/discussion.” Nutrition Reviews, June, 188-191, 2000.
[45]	Stanley J., “How good is the evidence that high intakes of trans fatty acids promote cardiovascular disease?” Lipid Technology, 11(6), 136-139, 1999.
[46]	Ackman R. G. & Burgher R. D., “A proposed basis for the systematic identification of unsaturated fatty acid esters through gas-liquid chromatography on polyester substances.” J. Chromatography, 11, 185-194, 1963.
[47]	Hayakawa K., Linko Y.-Y., & Linko P., “The role of trans fatty acids in human nutrition.” European Journal of Lipid Science and Technology,, 102(6), 419-425, 2000.
[48]	Chen Z. Y., Kwan K. Y., Tong K. K., Ratnayake W. M. N., Li H. Q. & Leung S. S. F., “Breast milk fatty acid composition: A comparative study between Hong Kong and Chongqing Chinese.” Lipids, 32, 1061-1067, 1997.
[49]	Wolff R. L., “Simple methods for the identification and quantification by GLC of most individual trans-18:1 isomers present in foods and human tissue.” Lipid Technology, 5 (1), 16-18, 1999.
[50]	Brakstad F., “Accurate determination of double bond position in mono-unsaturated straight-chain fatty acid ethyl esters from conventional electron impact mass spectra by quantitative spectrum-structure modeling.” Chem. Int. Lab. Syst., 19, 87-100, 1993.
[51]	Svein A. M. & Jan P., “Improved methods for analysis of fatty acid isomers.” Norwegian Herring oil and meal industry research institute”, 175 pp., 2001.
[52]	Fritsche J., & Steinhart H., “Contents of trans fatty acids (TFA) in German foods and estimation of daily intake.” Fett/Lipid, 99 (9), 314-318, 1997.
[53]	Duchateau G. S. M. J. E., van Oosten H. J., & Vasconcellos M. A., “Analysis of cis- and trans-fatty acid isomers in hydrogenated and refined vegetable oils by capillary gas-liquid chromatography.” JAOCS, 73 (3), 275-282, 1996.
[54]	FAO, “Fats and fatty acids in human nutrition.” Report of an expert consultation. FAO food and nutrition paper 91, 180 pp., 2008.
[55]	Folch J., Lees M. & Sloane-Stanley G. H., “A simple method for isolation and purification of total lipids from animal tissues.” J. Biol. Chem., 226: 497-509, 1957.
[56]	Bligh E. G. & Dyer W. J., “A rapid method of total lipid extraction and purification.” Can. J. Biochem. Physiol., 37: 911-917, 1959.
[57]	Marangoni F., Colombo C. & Galli C., “A method for the direct evaluation of the fatty acid status in a drop of blood from a fingertip in humans: applicability to nutritional and epidemiological studies.” Anal. Biochem., 326: 267-272, 2004a.
[58]	Gibon V., Ayala J., Dijckmans P., Maes J. & De Greyt W., “Future prospects for palm oil refining and modifications.” OCL, 16 (4): 193-200, 2009.
[59]	Mozzon M., Pacetti D., Lucci P., Balzano M. & Frega N. G., 2013. “Crude palm oil from interspecific hybrid Elaeis oleifera x Elaeis guineensis: Fatty acid regiodistribution and molecular species of glycerides.” Food Chemistry, 141: 245-252, 2013.
[60]	Alabi K. A., Lajide L. & Owolabi B. J., “Analysis of Fatty Acid Composition of Thevetia peruviana and Hura crepitans Seed oils using GC-FID. Fountain Journal of Natural and Applied Sciences, 2 (2): 32 - 37, 2013.
[61]	Oladimeji M. O., Akanni M. S., & Afolabi O. A., “Analysis of fatty acids extracted from Edible oils.” Nigerian Journal of Sciences, 25, 141-144, 1991.
[62]	Hardon J. J. & Tan G. Y., “Interspecific hybrids in the genus Elaeis. I. Crossability, cytogenetics and fertility of F1 hybrids of E. guineensis x E. oleifera.” Euphytica, 18 (3), 372-379, 1969.
[63]	Mir P. S., Bittman S., Hunt D., Entz T. & Yip B., “Lipid content and fatty acid composition of grasses sampled on different dates through the early part of the growing season.” Canadian Journal of Animal Science, 86: 279-290, 2006.
[64]	Purcell R., Latham S. H., Botham K. M., Hall W. L., & Wheeler-Jones C. PD., “High-fat meals rich in EPA plus DHA compared with DHA only have differential effects on postprandial lipemia and plasma 8-isoprostane F2a concentrations relative to a control high–oleic acid meal: a randomized controlled trial.” American Journal of Clinical Nutrition, 100: 1019-1028, 2014.
[65]	Applegate B. L., “Extraction, Derivatization, and Analysis of Fatty Acid Methyl Ester (FAME) in Tissue Homogenates and Blubber by ASE and Gas Chromatography.” Short description of FAME Analysis. Applied Science, Engineering, and Technology Laboratory, University of Alaska Anchorage, 11 pp., 2007.