Validasi Metode Analisis Kadar Arsen dalam Susu Bubuk dengan Destruksi Basah menggunakan ICP-MS

Abstract

Validasi metode perlu dilakukan terhadap metode analisis yang dimodifikasi. Penelitian ini bertujuan memvalidasi metode analisis kadar arsen dalam susu bubuk dengan metode standar Food and Drug Administration (FDA) Edisi 1.2 Tahun 2020 tentang Elemental Analysis in Food Using Microwave Assisted Digestion yang dimodifikasi pada penggunaan larutan pendestruksi. Validasi metode menghasilkan selektivitas sebesar 75 (m/z), batas deteksi instumen (BDI) sebesar 0,0080 µg/L, batas deteksi (BD) sebesar 24,70 µg/kg dan batas kuantitasi (BK) sebesar 82,32 µg/kg. Linearitas metode menghasilkan koefisien determinasi (R2) sebesar 0,9996. Presisi keterulangan memenuhi syarat keberterimaan %SBR < 2/3 CV Horwitz dan presisi antara memenuhi syarat keberterimaan uji t. Akurasi memenuhi syarat keberterimaan %recovery berada pada rentang 80% - 120%. Metode tahan terhadap perubahan volume larutan pendestruksi dan metode tangguh terhadap perubahan hari pengukuran. Metode modifikasi dinyatakan valid untuk analisis kadar arsen dalam susu bubuk karena memenuhi seluruh syarat keberterimaan, sehingga dapat digunakan untuk metode analisis rutin.

Method validation needed to be carried out on the modified analysis method. This study aimed to validate the analysis method of arsenic levels in powdered milk using the standard method of the Food and Drug Administration (FDA) Edition 1.2 of 2020 concerning Elemental Analysis in Food using Microwave Assisted Digestion modified by using a destructor solution. Method validation resulted in a selectivity of 75 (m/z), an instrument detection limit (IDL) of 0.0080 µg/L, a detection limit (DL) of 24,70 µg/kg and a quantitation limit (QL) of 82,32 µg/kg. The linearity of the method resulted in a determination coefficient (R2) of 0.9996. The repeatability precision met the acceptance requirements of %SBR <2/3 CV Horwitz and the intermediate precision met the acceptance requirements of the t test. The accuracy met the acceptance requirements %recovery in the range of 80% - 120%. The method was robust to changes in the volume of the destructive solution and the method was rugged to changes in the day of measurement. The modified method was declared valid for the analysis of arsenic levels in powdered milk because it met all the acceptance requirements, so it could be used for routine analysis methods.