Analisis Residu Pestisida Sulfoxaflor pada Pala (Myristica fragrans) Menggunakan LC MS/MS

Abstract

Analisis residu pestisida pada pala (Myristica fragrans) yang berpotensi mengandung residu pestisida sulfoxaflor sangat penting. Penelitian ini bertujuan untuk mengembangkan dan memvalidasi metode uji residu sulfoxaflor pada matriks pala menggunakan instrumen LC-MS/MS dan merumuskan instruksi kerja sebagai pedoman di laboratorium. Preparasi sampel dilakukan menggunakan metode ekstraksi QuEChERS, setelah itu dilanjutkan dengan pengujian menggunakan LC-MS/MS. Metode validasi menggunakan guideline SANTE/11312/2021 melalui parameter linearitas, efek matriks, limit of detection (LOD), limit of quantification (LOQ), akurasi, presisi, robustness, rasio ion, dan waktu retensi. Hasil penelitian menunjukkan linearitasnya sangat baik dengan nilai R² yaitu 0,9999 dan nilai back-calculated concentration 0,18% dan 0,10% pada hari pertama dan kedua. Nilai efek matriks menunjukkan ion suppression sebesar -77,73%, nilai signal-to-noise ratio pada LOD berada pada rentang 16–28,5, LOQ menunjukkan nilai presisi sebesar 7,72%, recovery sebesar 104,97%. Parameter presisi dan robustness memenuhi kriteria SANTE, yaitu =20%, sehingga metode dinyatakan valid dan layak digunakan untuk analisis residu sulfoxaflor pada matriks pala.

Pesticide residue analysis in nutmeg (Myristica fragrans) that potentially contains sulfoxaflor pesticide residues is crucial. This study aims to develop and validate a sulfoxaflor residue test method in nutmeg matrix using an LC-MS/MS instrument and formulate work instructions as laboratory test guidelines. Sample preparation was carried out using the QuEChERS extraction method, followed by testing using LC-MS/MS. The validation method used the SANTE/11312/2021 guidelines through parameters of linearity, matrix effect, limit of detection (LOD), limit of quantification (LOQ), accuracy, precision, robustness, ion ratio, and retention time. The results showed excellent linearity with an R² value of 0.9999 and back-calculated concentration values of 0.18% and 0.10% on the first and second days. The matrix effect value showed ion suppression of -77.73%, the signal-to-noise ratio value at LOD was in the range of 16–28.5, the LOQ showed a precision value of 7.72%, and the recovery was 104.97%. The precision and robustness parameters met the SANTE criteria, which was =20%, so the method was declared valid and suitable for use in the analysis of sulfoxaflor residues in nutmeg matrices.