Judul: Verifikasi Metode Analisis Senyawa Kontaminan 3- Mcpd Ester Dalam Minyak Sawit Dengan Teknik Gas Chromatography-Mass Spectrometry (Gc-Ms)
Abstrak: Senyawa 3-mono-chloropropane-1,2-diol (3-MCPD) ester merupakan senyawa kontaminan yang banyak ditemukan pada minyak sawit yang mengalami pemurnian. Tujuan dilakukan penelitian ini yaitu untuk melakukan verifikasi metode analisis 3-MCPD ester yang telah dilakukan oleh Lanovia (2013) untuk laboratorium pemerintah Badan POM, Jakarta. Kuantifikasi kandungan 3-MCPD ester dilakukan dengan menghitung selisih antara kandungan 3-MCPD total dan 3-MCPD bebas. Analisis dilakukan menggunakan instrumen Gas Chromatography-Mass Spectrometer (GC-MS) dan standar internal 3-MCPD-D5. Senyawa analat 3-MCPD dan 3-MCPD-D5 diderivatisasi oleh phenylboronic acid (PBA) menjadi senyawa yang dapat dideteksi oleh instrumen GC-MS yang masing-masing muncul pada menit ke- 16.476 – 17.065 dan 16.402 – 16.996 dengan presisi waktu retensi kurang dari 2.0 %. Hasil unjuk kerja instrumen menunjukkan instrumen memiliki linearitas yang baik pada rentang konsentrasi 3- MCPD 0.25 – 7.50 μg/mL dengan nilai R2 0.999. Nilai limit deteksi (LOD) dan limit kuantifikasi (LOQ) instrumen diperoleh masing-masing sebesar 0.17 dan 0.59 μg/mL. Hasil verifikasi menunjukkan metode analisis memiliki spesifisitas yang baik serta linieritas metode dengan nilai R2 0.995 pada rentang konsentrasi 3-MCPD 0 – 60 μg/g sampel. Nilai limit deteksi metode yang diperoleh adalah 4.59 μg/g. Hasil uji rekoveri pada konsentrasi spike 40 μg/g sampel diperoleh rata-rata rekoveri sebesar 83.29 ± 7.12 % pada rentang 77.89 – 96.49 % dan presisi yang baik yaitu sebesar 5.38 %. Nilai intralab reprodusibilitas yang diperoleh cukup baik dengan nilai RSD 7.70 %. Berdasarkan hasil tersebut maka metode analisis 3-MCPD ester yang telah terverifikasi dinyatakan valid. Pengujian 14 sampel minyak goreng sawit komersial menunjukkan 100 % sampel positif mengandung 3-MCPD ester yang berada pada rentang konsentrasi 8.15 – 58.14 μg/g minyak.
Keyword: 3-MCPD ester, 3-MCPD, verifikasi, minyak sawit

Judul: Validasi Metode Weihaar yang Dimodifikasi untuk Analisis 3-Monochloropropane-1,2-Diol (3-MCPD) dan Esternya pada Minyak Goreng Sawit
Abstrak: Food safety problems may occur throughout the food chain from farm to fork. Food Law (law No. 18, 2012) stated that food safety is condition and efforts needed to prevent food from contamination of biological, chemical and other agents, that may interfere, harm, and harmful to human health and do not contradict with religions, beliefs, and culture of the society so that it will be safe to be consumed. The compound of 3-monochloropropane-1,2-diol (3-MCPD) and its ester are contaminants formed during the food processing. Both of these compounds are found in vegetables oil and some processed food, especially food processed using heat in the production process. The mechanism of 3-MCPD formation and its esters has not been fully established. It has been hypothesized that 3-MCPD was formed by reaction between chlorine and lipids during cooking and storage process of food, that may be trigered by heat or enzyme-catalyzed reaction. Consequently, validated analytical method for analysis of 3-MCPD and its ester is needed. The research aims were to validate the modified Weihaar's method of analysis of 3-MCPD and 3-MCPD esters in refined palm oil. The research was conducted in three main stages including determining the analysis method to determine the levels of 3-MCPD and its esters in palm oil using GC-MS; validation of analysis methods; and determining the levels of 3-MCPD in several product of palm oil. Validation result shows the following: A linear regression line has an equation of the form y = 0.076x + 0.005, where x is area ratio of standard external and standard internal and y is concentration ratio of external standard and internal standard. The linearity was showed by corelation coefficient (r) 0.994; linear response was obtained between 0.008 and 0.377 mg/L; limit of detection was 0.06 mg/kg, limit of quantification was 0.20 mg/kg, precision (relative standard deviation (RSD)) was 6.16%, and accuracy (as percentage of recovery) was in range 95.83-113.27%. This result indicated that the modified method was valuable and sensitive for detection of 3-MCPD and 3-MCPD esters. Using the validated method, the 3-MCPD esters in commercial palm oil sample determined and calculated as the difference between total 3-MCPD and free 3-MCPD, was 13.24 mg/kg. The total 3-MCPD in several palm oil give result on concentration range 13.94-34.52 mg/kg. These results also showed that there was a correlation between 3-MCPD with diacylglyceride (DAG). The sampel with high DAG contents give a high test results of 3-MCPD, this relationship was expressed by the coefficient of correlation (r) 0.752.
Keyword: 3-MCPD, 3-MCPD esters, validation methods, GC-MS

Judul: Embriogenesis ikan buta (Astyanax fasciatus)
Abstrak: Ikan buta Astyanax fasciatus adalah spesies ikan unik dari famili Characidae yang menempati perairan dalam gua di Wilayah La Cueva Chica-San Luis Potasi-Mexico. Ikan ini memiliki mata yang tereduksi (Blind Cavefish) dan warna kulit merah muda, pucat serta mengkilap.
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