Validasi Metode Analisis Kadar Kalsium pada Susu Segar secara Titrasi Kompleksometri

https://doi.org/10.22146/agritech.25459

Moh. Taufik(1*), Seveline Seveline(2), Emilia Ratih Saputri(3)

(1) Program Studi Ilmu dan Teknologi Pangan, Fakultas Bioindustri, Universitas Trilogi, Jl. TMP, Kalibata No. 1, Jakarta Selatan 12760
(2) Program Studi Ilmu dan Teknologi Pangan, Fakultas Bioindustri, Universitas Trilogi, Jl. TMP, Kalibata No. 1, Jakarta Selatan 12760
(3) Program Studi Ilmu dan Teknologi Pangan, Fakultas Bioindustri, Universitas Trilogi, Jl. TMP, Kalibata No. 1, Jakarta Selatan 12760
(*) Corresponding Author

Abstract


Analysis of calcium content in fresh milk generally uses Atomic Absorption Spectroscopy (AAS). Alternatively, it could be analyzed using complexometric titration. The study aimed to validate the method of calcium content analysis in fresh milk by complexometric titration. The results showed that the linearity test using calcium standard solution at a working range of 4-24 mg/100 mL had R2 of 0.9983, while the limit of detection and limit of quantification were 0.47 mg/100 mL and 1.57 mg/100 mL, respectively. The accuracy by spiking method at the spiking concentration of 60 mg/100 mL sample was 99.29%. The repeatability and intra-lab reproducibility showed acceptable precision with CV value of 0.98% and 2.59%, respectively. The results of ruggedness test showed that this method was rugged to the variation of sample volume and ethylenediaminetetraacetic acid (EDTA) concentration. This study proved that complexometric titration can be used to determine calcium content in fresh milk.

 

ABSTRAK

Analisis kadar kalsium pada susu segar umumnya menggunakan Atomic Absorption Spectroscopy (AAS) yang relatif mahal. Salah satu metode alternatif yang dapat digunakan adalah titrasi kompleksometri. Sampai sekarang, data validasi terhadap metode tersebut pada sampel susu segar belum tersedia. Tujuan penelitian ini adalah memvalidasi metode analisis kadar kalsium pada susu segar secara titrasi kompleksometri. Hasil penelitian menunjukkan uji linearitas dengan menggunakan larutan standar kalsium pada rentang 4-24 mg/100 mL mempunyai nilai R2 sebesar 0,9983, sedangkan nilai batas deteksi dan batas kuantifikasi berturut-turut adalah 0,47 mg/100 mL dan 1,57 mg/100 mL. Nilai akurasi (recovery) sebesar 99,29% pada konsentrasi spiking 60 mg/100 mL sampel. Hasil penelitian atau metode uji yang divalidasi menunjukkan nilai keterulangan dan reprodusibilitas intralab yang baik dengan nilai CV analisis berturut-turut 0,98% dan 2,59%. Hasil uji ketangguhan menunjukkan metode ini bersifat tangguh (rugged) terhadap variasi volume sampel dan konsentrasi asam etilenadiaminatetraasetat (EDTA) yang digunakan. Berdasarkan hasil penelitian tersebut, metode titrasi kompleksometri dapat digunakan untuk menentukan kadar kalsium pada susu segar. 

 


Keywords


Calcium analysis; complexometric titration; fresh milk; method validation

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References

Al-Wabel, N. A. (2008). Mineral contents of milk of cattle, camels, goats and sheep in the central region of Saudi Arabia. Asian Journal of Biochemistry, 3(6), 373–375. http://doi.org/10.3923/ajb.2008.373.375

AOAC. (2012). Official Methods of Analysis of AOAC International (19th ed.). Maryland, MD: AOAC International Press

Baldut, M., Bonafede, S. L., Petrone, L., Simionato, L. D., & Segall, A. I. (2015). Development and validation of a complexometric titration method for the determination of rosuvastatin calcium in raw material. Advances in Research, 5(5), 1-8. http://doi.org/10.9734/AIR/2015/19843

Barłowska, J., Szwajkowska, M., Litwińczuk, Z., & Król, J. (2011). Nutritional value and technological suitability of milk from various animal species used for dairy production. Comprehensive reviews in food science and food safety, 10(6), 291-302. https://doi.org/10.1111/j.1541-4337.2011.00163.x

Basak, S., & Kundu, D. (2013). Evaluation of measurement uncertainty components associated with the results of complexometric determination of calcium in ceramic raw materials using EDTA. Accreditation and Quality Assurance, 18(3), 235-241.

Beto, J. A. (2015). The role of calcium in human aging. Clinical nutrition research, 4(1), 1-8. https://doi.org/10.7762/cnr.2015.4.1.1

BSN. (2004). SNI 06-6989 13-2004. Air dan Air Limbah. Jakarta: Badan Standarisasi Nasional

Budiman, S., Nugroho, P., & Fudiesta, Y. (2013). Studi penentuan kandungan kalsium dan kemungkinan terkontaminasinya logam timbal dalam susu sapi secara spektrofotometri serapan atom (SSA). Aristoteles, 10(2), 16-22.

Česnik, H. B., & Gregorčič, A. (2006). Validation of the method for the determination of dithiocarbamates and thiuram disulphide on apple, lettuce, potato, strawberry and tomato matrix. Acta Chimica Slovenica, 53(1), 100-104.

Cai, J. B., Wang, S. F., Tang, P. P., & Su, Q. D. (2009). Simultaneous determination of total nitrogen and metal elements in tobaccos by high performance ion chromatography. Journal of the Chinese Chemical Society, 56(4), 671-675. https://doi.org/10.1002/jccs.200900100

Dandare, S. U., Ezeonwumelu, I. J., & Abubakar, M. G. (2014). Comparative analysis of nutrient composition of milk from different breeds of cows. Scholars Research Library European Journal of Applied Engineering and Scientific Research, 3(2), 33-36.

Day, R. A. & Underwood, A. L. (2006). Analisis Kimia Kuantitatif (6th ed). Jakarta: Erlangga

Depkes RI. (2005). Daftar Komposisi Bahan Makanan. Jakarta: Departemen Kesehatan Republik Indonesia

Gobinathan, P., Murali, P. V., & Panneerselvam, R. (2009). Interactive effects of calcium chloride on salinity-induced proline metabolism in Pennisetum typoidies. Advances in Biological Research, 3(5-6), 168-173.

Harmita, H. (2012). Petunjuk pelaksanaan validasi metode dan Cara Perhitungannya. Pharmaceutical Sciences and Research (PSR), 1(3), 117-135. https://doi.org/10.7454/psr.v1i3.3375

Janagiraman, S., Raju, T., & Giribabu, K. (2014). Simple Titrimetric Analysis for Determination of Pitavastatin Calcium in Bulk and Formulation Dosage. Int. J. Modern Chem, 6(1), 18-27.

Kantasubrata, J. (2008). Validasi Metode. Bandung: Pusat Penelitian LIPI

Kapadnis, K. H. (2015). Magnesium and calcium estimation from fresh milk samples in nashik region by a simple method. World Journal of Pharmacy And Pharmaceutical Sciences, 4(12), 793-797

Kazusaki, M., Ueda, S., Takeuchi, N., & Ohgami, Y. (2012). Validation of analytical procedures by high− performance liquid chromatography for pharmaceutical analysis. Chromatography, 33(2), 65-73. https://doi.org/10.15583/jpchrom.2012.005

Kumaravel, S., & Alagusundaram, K. (2014). Determination of mineral content in Indian spices by ICP-OES. Oriental journal of chemistry, 30(2), 631-636. http://dx.doi.org/10.13005/ojc/300231

Looper, M. (2012). Factors Affecting Milk Composition of Lactating Cows. Arkansas: University of Arkansas

Miefthawati, N. P., Gusrina, L., & Axela, F. (2013). Penetapan kadar kalsium pada ikan kembung segar dan ikan kembung asin secara kompleksometri. Jurnal Analisis Kesehatan Klinikal Sains, 1(1), 1-9.

Nielsen, S. S. (2010). Complexometric Determination of Calcium. In Nielsen, S.S. (Ed.). Food analysis laboratory manual (pp. 61-67). New York, NY: Springer.

Park, Y. W., Juárez, M., Ramos, M., & Haenlein, G. F. W. (2007). Physico-chemical characteristics of goat and sheep milk. Small ruminant research, 68(1), 88-113. https://doi.org/10.1016/j.smallrumres.2006.09.013

Petrovich, M. B., Filho, V. R. A., & Neto, J. A. G. (2007).  Direct determination of calcium in milk by atomic absorption spectrometry using flow-injection analysis. Eclética Química, 32(3), 25-30. http://dx.doi.org/10.1590/S0100-46702007000300004 

Poirier, L., Nelson, J., Leong, D., Berhane, L., Hajdu, P., & Lopez-Linares, F. (2016). Application of ICP-MS and ICP-OES on the determination of nickel, vanadium, iron, and calcium in petroleum crude oils via direct dilution. Energy & Fuels, 30(5), 3783-3790. http://dx.doi.org/10.1021/acs.energyfuels.5b02997

Pratama, D. S., Pirdaus, P., Rinawati, R., Sagala, S. L., & Suhelmi, I. S. R. (2015). Validasi metode analisis logam Na, K, Mg dan Ca pada air tua (bittern) menggunakan Microwave Plasma-Atomic Emission Spectrometer (MP-AES). Jurnal Standardisasi, 17(3), 187-198. http://dx.doi.org/10.31153/js.v17i3.318

Riyanto. (2014). Validasi dan Verifikasi Metode Uji. Yogyakarta: Deepublish Publisher

Rusdi, R., Maryesri, M., & Zulharmitta, Z. (2013). Pembuatan Kalsium Karbonat Dari Batu Kapur Bukit Tui Kota Padang Panjang. Jurnal Farmasi Higea, 5(2), 159-166.

Setyawan, A. A., Mustofa, C. H., & Hidayat, R. (2017). Pengaruh perebusan terhadap kadar kalsium pada bayam hijau (amaranthus tricolor, L) dengan metode kompleksometri. Motorik, 12(24), 75-83.

Sowmya, R., Indumathi, K. P., Arora, S., Sharma, V., & Singh, A. K. (2015). Detection of calcium based neutralizers in milk and milk products by AAS. Journal of food science and technology, 52(2), 1188-1193.

Squadrone, S., Ferro, G. L., Marchis, D., Mauro, C., Palmegiano, P., Amato, G., ... & Abete, M. C. (2010). Determination of melamine in feed: validation of a gas chromatography–mass spectrometry method according to 2004/882/CE regulation. Food Control, 21(5), 714-718. https://doi.org/10.1016/j.foodcont.2009.10.013

Ward, R. E., & Carpenter, C. E. (2010) Traditional Methods for Mineral Analysis. In Nielsen, S. S. (Ed). Food analysis 4th (pp. 201-2015). New York, NY: Springer

Wenclawiak, B., & Hadjicostas, E. (2010). Validation of Analytical Methods–to be Fit for the Purpose. In Wenclawiak, Bernd W., Koch, M., & Evsevios, H. (Eds.). Quality Assurance in Analytical Chemistry (pp. 215-245). Berlin Heidelberg: Springer

Zamberlin, Š., Antunac, N., Havranek, J., & Samaržija, D. (2012). Mineral elements in milk and dairy products. Mljekarstvo/Dairy, 62(2), 111-125



DOI: https://doi.org/10.22146/agritech.25459

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