Verification of The Method for Determining Calcium Content in Animal Feed
DOI:
https://doi.org/10.22437/chp.v9i2.48076Kata Kunci:
Animal feed, calcium, ICP-OES, method verificationAbstrak
Calcium is one of the essential macromineral elements in animal feed. To ensure that animal feed meets nutritional and safety standards, accurate and validated analytical methods are needed to determine calcium levels, specifically using the ICP-OES (Inductively Coupled Plasma Optical Emission Spectroscopy) technique, which is known for its high sensitivity, enabling the rapid and precise detection of calcium elements at low concentrations. This study aims to verify the method for analyzing calcium content in animal feed, referring to method verification parameters, including linearity, accuracy, precision (repeatability test), limit of detection (LoD), method detection limit (MDL), and limit of Quantitation (LOQ). The verification process was conducted using calcium standard solutions at various concentrations and analysis of animal feed samples according to SNI 3148.2:2009 using Inductively Coupled Plasma (ICP-OES) with a linearity test parameter coefficient of correlation (r) value of 0.9991, precision with a % RSD value of 2.18%, accuracy (recovery) reaches 90-99%, with a detection limit (LoD) of 0.0745 mg/L and a Limit of Quantitation (LoQ) of 0.9060 mg/L, all of which meet the acceptance criteria set by AOAC. These results prove that the ICP-OES technique is suitable for use as a test method for determining the calcium content in animal feed, can be adopted as a standardized routine procedure.
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[1]. Moorby, J. M., & Fraser, M. D. New feeds and new feeding systems in intensive and semi-intensive forage-fed ruminant livestock systems: A review. Animal, 2021. 15: 100297.https://doi.org/10.1016/j.animal.2021.100297
[2]. Sonea, C., Gheorghe-Irimia, R.-A., Tăpăloagă, D., & Tăpăloagă, P.-R. Nutrition and animal agriculture in the 21st century: A review of future prospects. Annals of the University of Craiova – Agriculture, Montanology, Cadastre Series, 2023. 53(1): 303–312. https://doi.org/10.52846/aamc.v53i1.1482
[3]. Malik, D., Narayanasamy, N., Pratyusha, V. A., Thakur, J., & Sinha, N. Inorganic nutrients: Macrominerals. In Textbook of Nutritional Biochemistry, 2023. 391–446. https://doi.org/10.1007/978-981-19-4150-4_11
[4]. Wu, G. Management of metabolic disorders (including metabolic diseases) in ruminant and non-ruminant animals. In Animal Agriculture. 2020. 471–491). https://doi.org/10.1016/B978-0-12-817052-6.00027-6
[5]. Carter, S., Clough, R., Fisher, A., Gibson, B., Russell, B., & Waack, J. Atomic spectrometry update: Review of advances in the analysis of metals, chemicals and materials. Journal of Analytical Atomic Spectrometry, 34(11): 2159–2216. 2019. https://doi.org/10.1039/C9JA90058F
[6]. Khan, S. R., Sharma, B., Chawla, P. A., & Bhatia, R. Inductively coupled plasma optical emission spectrometry (ICP-OES): A powerful analytical technique for elemental analysis. Food Analytical Methods, 2022. 15(3): 666–688. https://doi.org/10.1007/s12161-021-02148-4
[7]. Zhang, J. The role of verification and validation process in best estimate plus uncertainty methodology development. Nuclear Engineering and Design, 355: 110312. 2019. https://doi.org/10.1016/j.nucengdes.2019.110312
[8]. Oreste, E. Q., et al. Evaluation of sample preparation methods for the determination of Ca, Cu, Fe, K, and Na in milk powder samples by ICP-OES. Food Analytical Methods, 2016. 9(3): 777–784. https://doi.org/10.1007/s12161-015-0252-1
[9]. Phan-Thien, K.-Y., Wright, G. C., & Lee, N. A. Determination of essential minerals in peanuts by ICP-MS and ICP-OES. Food Chemistry, 2012. 134(1): 453–460. https://doi.org/10.1016/j.foodchem.2012.02.095
[10]. Kargarghomsheh, P., et al. Evaluation of elements in Persian tahini using ICP-OES. International Journal of Environmental Analytical Chemistry, 2025. 105(8): 1723–1737. 2025. https://doi.org/10.1080/03067319.2023.2298363
[11]. Düzgün, M., & Kahraman, Ş. Evaluation of mineral safety index, nutritional and risk assessment of sorghum genotypes using ICP-OES. Journal of Food Composition and Analysis, 2025. 146: 107960. https://doi.org/10.1016/j.jfca.2025.107960
[12]. Betz, J. M., Brown, P. N., & Roman, M. C. Accuracy, precision, and reliability of chemical measurements in natural products research. Fitoterapia, 2010. 82(1): 44–52. 2011. https://doi.org/10.1016/j.fitote.2010.09.011
[13]. Jurado, J. M., Alcázar, A., Muñiz-Valencia, R., Ceballos-Magaña, S. G., & Raposo, F. Practical considerations for linearity assessment of calibration curves. Talanta, 2017. 172: 221–229. 2017. https://doi.org/10.1016/j.talanta.2017.05.049
[14]. McAlinden, C., Khadka, J., & Pesudovs, K. Precision (repeatability and reproducibility) studies and sample-size calculation. Journal of Cataract and Refractive Surgery, 2015. 41(12): 2598–2604. 2015. https://doi.org/10.1016/j.jcrs.2015.06.029
[15]. Mehl, A., Reich, S., Beuer, F., & Güth, J. F. Accuracy, trueness, and precision: A guideline for digital dentistry. International Journal of Computerized Dentistry, 2021. 24(4): 341–352.
[16]. Riviere, J. E. Chemistry and limits of analytical detection and quantitation. In Zero – Much to Do About Nothing? (pp. 85–102). https://doi.org/10.1007/978-3-031-82998-7_6
[17]. Aldakheel, R. K., Gondal, M. A., Nasr, M. M., Almessiere, M. A., & Idris, N. Spectral analysis of Moringa oleifera leaves using XPS, LIBS and ICP-OES. Talanta, 2020. 217: 121062. 2020. https://doi.org/10.1016/j.talanta.2020.121062
[18]. Rehan, I., Gondal, M. A., Rehan, K., & Sultana, S. Spectral diagnosis of toxic elements in face powders using LIBS and ICP-OES. Talanta, 2020. 217: 121007. https://doi.org/10.1016/j.talanta.2020.121007
[19]. Jarantow, S. W., Pisors, E. D., & Chiu, M. L. Linear and nonlinear regression analysis in quantitative biological assays. Current Protocols, 2023. 3(6). 2023. https://doi.org/10.1002/cpz1.801
[20]. Stalikas, C., & Sakkas, V. Calibration and correlation in chemical analysis: Practical considerations. Microchimica Acta, 2024. 191(2): 81. https://doi.org/10.1007/s00604-023-06157-4
[21]. Hazra, A., & Gogtay, N. Correlation and linear regression. Indian Journal of Dermatology, 2016. 61(6): 593. 2016. https://doi.org/10.4103/0019-5154.193662
[22]. Brunetti, D. E. About estimating the limit of detection by the signal-to-noise approach. Pharmaceutical Analytical Acta, 2015. 6(4). 2015. https://doi.org/10.4172/2153-2435.1000355
[23]. González, A. G., & Herrador, M. Á. Practical guide to analytical method validation. TrAC Trends in Analytical Chemistry, 2007. 26(3): 227–238. https://doi.org/10.1016/j.trac.2007.01.009
[24]. Lestari, S., Watini, S., & Rose, D. E. Impact of self-efficacy and work discipline on employee performance. Aptisi Transactions on Technopreneurship, 2024. 6(2): 270–284.https://doi.org/10.34306/att.v6i2.403
[25]. Prenesti, E., & Gosmaro, F. Trueness, precision and accuracy: A critical overview. Accreditation and Quality Assurance, 2015. 20(1): 33–40. 2015. https://doi.org/10.1007/s00769-014-1093-0
[26]. Nair, A., Chandrashekhar, H. R., & Nayak, U. Y. RP-HPLC method for quantification of cefotaxime sodium using green analytical approach. Journal of Applied Pharmaceutical Science. 2024. https://doi.org/10.7324/JAPS.2024.192430
[27]. Feinberg, M. Validation of analytical methods based on accuracy profiles. Journal of Chromatography A, 2007. 1158(1–2): 174–183. https://doi.org/10.1016/j.chroma.2007.02.021
[28]. Taleuzzaman, M. Limit of blank, limit of detection and limit of quantification. Organic & Medicinal Chemistry International Journal, 2018. 7(5). https://doi.org/10.19080/OMCIJ.2018.07.555722
[29]. Bulska, E., & Ruszczyńska, A. Analytical techniques for trace element determination. Physical Sciences Reviews, 2017. 2(5). https://doi.org/10.1515/psr-2017-8002
[30]. Gegenschatz, S. A., Chiappini, F. A., Teglia, C. M., Muñoz de la Peña, A., & Goicoechea, H. C. Computing limits of detection and quantification in univariate calibration. 2022. Analytica Chimica Acta, 1209: 339342. https://doi.org/10.1016/j.aca.2021.339342
[31]. Khamis, M. M., Adamko, D. J., & El-Aneed, A. Method development and validation for absolute quantification of endogenous metabolites. Mass Spectrometry Reviews, 2021. 40(1): 31–52. https://doi.org/10.1002/mas.21607
[32]. Ehling, S., Thompson, J. J., Schimpf, K. J., Pacquette, L. H., & Haselberger, P. A. Precision of modern analytical methods in food analysis. Journal of AOAC International, 108(4): 566–571. 2025. https://doi.org/10.1093/jaoacint/qsaf026
[33]. Peters, F. T., & Maurer, H. H. Bioanalytical method validation in forensic and clinical toxicology. Accreditation and Quality Assurance, 7(11): 441–449. 2002. https://doi.org/10.1007/s00769-002-0516-5
[34]. Uhrovčík, J. Strategy for determination of LOD and LOQ values. Talanta, 119: 178–180. 2014. https://doi.org/10.1016/j.talanta.2013.10.061
[35]. Peris-Vicente, J., Esteve-Romero, J., & Carda-Broch, S. Validation of analytical methods based on chromatographic techniques. In Analytical Separation Science, 2015. 5, 1757–1808). https://doi.org/10.1002/9783527678129.assep064
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