Pengembangan dan Validasi Prosedur Pengukuran Logam Timbal (Pb) dalam Makanan Pendamping Air Susu Ibu Menggunakan Spektroskopi Serapan Atom

Abstract

Validasi metode analisis telah berhasil dilakukan untuk pengukuran logam timbal (Pb) dalam 5 jenis makanan pendamping air susu Ibu (MP-ASI). Logam timbal (Pb) dianalisis menggunakan spektroskopi serapan atom setelah didestruksi dengan asam nitrat dan dipanaskan menggunakan automatic digester pada suhu 130 oC dan lama pemanasan 60 menit.Tujuan dilakukan penelitian ini untuk menghasilkan suatu metode analisis baru yang lebih sederhana, mudah diaplikasikan, dan waktu analisis lebih cepat. Hasil penelitian menunjukkan bahwa semua sampel dengan kode SBM, SKI, CBM, CKI dan ProAKB terdapat logam timbal (Pb) dengan konsentrasi berturut-turut sebesar 0,87; 1,02; 1,44; 1,48 dan 2,00 mg/L. Tiga dari 5 sampel tersebut, memiliki konsentrasi Pb yang melebihi ambang batas SNI 7387:2009. Hasil pengembangan metode ini telah memenuhi persyaratan validasi seperti linieritas, akurasi, presisi, batas deteksi dan kuantisasi. Linieritas dikonfirmasi melalui larutan standar Pb 0,2 ‒ 1,0 mg/L dengan perolehan koefisien korelasi (r2) 0,9994, persen perolehan kembali 88,0 ‒ 95,1%, standar deviasi relatif (RSD) 5,7 ‒ 7,3%, batas deteksi (LOD) metode 0,007 sedangkan nilai batas kuantisasi (LOQ) sebesar 0,023 mg/L. Metode destruksi ini dapat dikategorikan sebagai metode preparasi yang tepat, teliti, sederhana dan dapat dijadikan sebagai metode analisis Pb pada sampel berbeda.

Improvement and Validation of Procedure to Measure Lead (Pb) In A Complementary Food for Breast Milk Using Atomic Adsorption Spectroscopy. Validation of the analytical method was successfully carried out for the measurement of lead (Pb) in 5 types of complementary foods for breast milk (MP-ASI). This element was measured by atomic absorption spectrometer after digested of the samples with nitric acid by automatic digester at 130 oC for 60 minutes. The purpose of this research is to develop a new measurement method that is simpler and faster analysis. The results showed that all samples with SBM, SKI, CBM, CKI and ProAKB codes contained of lead (Pb) 0.87; 1.02; 1.44; 1.48 and 2.00 mg/L respectively. Three of the 5 samples contained Pb levels that exceeded the SNI 7387:2009 threshold. The development of this method met the validation requirements such as linearity, precision, accuracy, detection and quantification limits (LOD and LOQ). Respons of linearity was verified for concentrations ranging from 0.2 to 1.0 mg/L of lead standard solution. Correlation coefficient (r2) of the calibration straight lines was 0.9994. Repeatability of the method gave relative standard deviation (RSD) of 5.7 ‒ 7.3%. The recovery of lead obtained after spiking method with increasing amounts of lead rate of 88.0 ‒ 95.1%. Limits of detection and quantification were 0.007 and 0.023 mg/L respectively. This method can be categorized as an appropriate, thorough, fast, and can be used in different samples.