VALIDASI METODE ANALISIS NITRIT DAN NITRAT DALAM DAGING SEGAR DAN PRODUK DAGING OLAHAN SECARA SPEKTROFOTOMETRI UV-VIS

FIRMAN SHANTYA BUDI, Drs.Roto,M.Eng.,Ph.D.

2014 | Tesis | S2 Ilmu Kimia

Validasi metode analisis nitrit dan nitrat dalam daging segar dan produk daging olahan secara spektrofotometri UV-Vis dengan pereaksi sulfanilamida dan N-naftiletilendiamina (NEDA) telah dilakukan. Nitrat direduksi menjadi nitrit menggunakan reduktor serbuk Zn. Optimasi metode analisis dilakukan sebelum validasi. Tahap selanjutnya metode divalidasi dengan pendekatan spiking buta nol berdasarkan parameter validasi meliputi linieritas, sensitivitas, batas deteksi, batas kuantifikasi, ketelitian dan ketepatan. Metode diaplikasikan untuk penentuan nitrit dan nitrat dalam daging segar dan produk daging olahan (sosis, daging asap dan kornet). Absorbansi senyawa azo mencapai optimum pada panjang gelombang 541 nm. Sementara itu, hasil validasi menunjukkan linieritas standar nitrit pada rentang 0,1 - 0,8 mg/L (R2= 0,9995) dengan absorptivitas molar sebesar 5,37 x 104 L mol-1 cm-1. Batas deteksi dan kuantifikasi masing-masing sebesar 0,021 dan 0,063 mg/L dengan %RSD analisis nitrit dan nitrat masing-masing sebesar 0,56 dan 1,73%. Persentase perolehan kembali analisis nitrit dan nitrat masing-masing antara 85 - 99% dan 82 - 100%. Konsentrasi nitrit dan nitrat yang ditentukan dalam daging masing-masing antara 0,60 - 14,79 mg/kg dan 0,68 - 8,39 mg/kg.

Validation of nitrite and nitrate analysis methods in fresh meat and meat product by UV-Vis spectrophotometry using sulfanilamide and N-naftyletilendiamine (NEDA) reagent was studied. Zinc powder was used as reducing agent to reduce nitrate to nitrite. The method was optimized in advance before validation. The method was validated by zero blind spiking approach based on various validation parameters such as linearity, sensitivity, limit of detection, limit of quantification, precision and accuracy. The method was applied for determining nitrite and nitrate in fresh meat and meat products (sausage, smoked beef and cornet). The azo compound absorbance reached the optimum level at 541 nm. Meanwhile, the validation results showed linearity nitrite standard in the range from 0.1 -0.8 mg / L (R2= 0.9995) with molar absorptivity 5.37 x 104 L mole-1 cm-1. The limit of detection and limit of quantification of the proposed method were 0.021 and 0.063 mg/L respectively with %RSD of nitrite and nitrate analysis were 0.56 and 1.73%, respectively. The percent recovery of nitrite and nitrate were 85 - 99% and 82 - 100%, respectively. The range of nitrite and nitrate concentration were 0.60 - 14.79 mg/kg dan 0.68 - 8.39 mg/kg, respectively.

Kata Kunci : nitrite, nitrate, sulfanilamide, NEDA, validation, UV-Vis spectrophotometry