Ni Nyoman Trisnawati, Ni Putu Ayu Krismayanti, Putu Primantari Vikana Suari

VALIDASI METODE UJI NITRIT MENGGUNAKAN SPEKTROFOTOMETER UV-VIS 2600

Introduction

validasi metode uji nitrit menggunakan spektrofotometer uv-vis 2600. Validasi metode uji Nitrit menggunakan Spektrofotometer UV-Vis 2600. Pastikan analisis akurat & terpercaya untuk nitrit dalam air/daging. Uji linieritas, LOD, LOQ, akurasi, presisi.

Abstract

ABSTRAK: Salah satu laboratorium yang menunjang kegiatan Tri Dharma Perguruan Tinggi di Universitas Udayana adalah Laboratorium Analitik. Laboratorium ini memberikan fasilitas dalam hal praktikum dan praktik kerja lapangan kepada mahasiswa, membantu penelitian mahasiswa maupun dosen, dan melayani masyarakat untuk uji sampel dalam bidang kimia dan fisika. Parameter yang sering diuji oleh mahasiswa, dosen, maupun masyarakat adalah Nitrit (NO2), yang biasanya terkandung dalam air dan daging olahan. Metode uji Nitrit dilakukan dengan menggunakan instrumen Spektrofotometer UV-Vis 2600 dengan larutan standar Nitrit yang dibuat dari senyawa Natrium Nitrit (NaNO2). Larutan standar ini belum bersertifikat (CRM), sehingga validasi standar perlu dilakukan untuk membuktikan bahwa larutan standar tersebut memenuhi persyaratan untuk digunakan dalam metode uji, dan data yang diperoleh dapat dipercaya serta akurat. Penelitian ini bertujuan untuk memastikan bahwa metode uji Nitrit menggunakan Spektrofotometer UV-Vis 2600 sudah valid. Manfaat penelitian ini adalah mendapatkan larutan standar Nitrit yang telah tervalidasi. Validasi metode yang digunakan meliputi uji linieritas, LOD, LOQ, akurasi, dan presisi. Hasil yang diperoleh adalah: nilai r sebesar 0,9995 yang menyatakan linier; nilai LOD dan LOQ adalah 0,0026 mg/L dan 0,0088 mg/L serta sudah terkonfirmasi, hasil uji akurasi (%Recovery) sudah masuk dalam rentang yang ditetapkan yakni 90-110%; dan hasil uji presisi sudah memiliki nilai %RSD < 2/3 CV Horwitz. Berdasarkan hasil penelitian yang sudah memenuhi persyaratan, dapat dinyatakan bahwa larutan standar Nitrit dari senyawa Natrium Nitrit (NaNO2) sudah valid digunakan dalam metode uji Nitrit.   ABSTRACT: One of the laboratories that work follows the three responsibilities of Higher Education at Udayana University is the Analytical Laboratory. This laboratory provides facilities in terms of practicum and field work practice to students, assists student and lecturer research, and serves clients outside Udayana University in the area of chemical and physical analysis. The parameter that is often tested by students, lecturers, and other clients is Nitrite (NO2), which is usually contained in water and processed meat. The nitrite test method was carried out using a Spectrophotometer UV-Vis 2600 instrument with a standard Nitrite solution made from the compound Sodium Nitrite (NaNO2). The standard solution has not been certified (CRM), so standard validation needs to be done to prove that the standard solution meets the requirements for use in the test method, and the data obtained is reliable and accurate. This research aims to ensure that the Nitrite test method using the Spectrophotometer UV-Vis 2600 is valid. The benefit of this research is to obtain a validated Nitrite standard solution. The method validation used includes linearity, LOD, LOQ, accuracy, and precision tests. The results obtained were: r value was 0,9995 which states linear; the value of LOD and LOQ were 0,0026 mg/L and 0,0088 mg/L respectively and they were already confirmed; result of accuracy (%Recovery) was in the range of 90-110%; and result of precision test was in %RSD < 2/3 CV Hortwitz. Based on the research results that have fulfilled the requirements, it can be stated that the standard solution of Nitrite from the compound Sodium Nitrite (NaNO2) is valid for use in the Nitrite test method.

Review

The submitted work, titled "VALIDASI METODE UJI NITRIT MENGGUNAKAN SPEKTROFOTOMETER UV-VIS 2600," addresses a critical aspect of analytical chemistry: method validation. The abstract clearly outlines the context within the Analytical Laboratory at Udayana University, which frequently analyzes nitrite (NO2) in samples like water and processed meat. The fundamental challenge identified is the reliance on an in-house prepared, non-certified sodium nitrite standard solution. This necessitates a robust validation to ensure the reliability and accuracy of analytical data, a crucial step for any laboratory supporting academic research, student training, and public service. The research systematically tackled this issue by performing a comprehensive validation of the nitrite test method utilizing a UV-Vis 2600 spectrophotometer. The validation parameters selected were appropriate and encompassed the essential characteristics of an analytical method: linearity, Limit of Detection (LOD), Limit of Quantitation (LOQ), accuracy, and precision. The reported results demonstrate strong performance across all criteria. Specifically, the linearity (r = 0.9995) indicates an excellent correlation, while the LOD (0.0026 mg/L) and LOQ (0.0088 mg/L) are well-defined. Crucially, the accuracy, expressed as %Recovery, fell within the acceptable range of 90-110%, and the precision, measured by %RSD, satisfied the stringent criterion of being less than 2/3 of the Horwitz CV. These findings collectively confirm that the method, employing the prepared standard solution, meets the necessary analytical requirements. This validation study represents a significant and valuable contribution to the Analytical Laboratory at Udayana University. By rigorously validating the nitrite test method and its associated standard solution, the research provides a strong foundation for producing dependable and accurate analytical results. This directly enhances the quality of data for student practicums, research projects by both students and lecturers, and services offered to the community. The successful validation ensures confidence in the analytical output, thereby strengthening the laboratory's capabilities and its adherence to good laboratory practice, which is vital for fulfilling the "Tri Dharma Perguruan Tinggi" responsibilities.

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