ANALISIS MULTI RESIDU ORGANOKLORIN PADA TELUR ITIK ASAL KABUPATEN BANTUL MENGGUNAKAN METODE QuEChERS DAN GAS CHROMATOGRAPHY - MASS SPECTROMETRY (GC-MS)

TRI WIDAYATI, Dr.drh. Doddi Yudhabuntara;Dr. drh. R. Gagak Donny Satria, M.P., M.Pd.

2015 | Tesis | S2 Sain Veteriner

Telur itik merupakan sumber protein hewani yang terjangkau oleh masyarakat, namun mempunyai potensi mengandung multi residu diantaranya residu pestisida organoklorin. Jaminan keamanan pangan yang didukung oleh pengujian laboratori yang valid diperlukan untuk menjamin bahan pangan aman, berkualitas, dan layak untuk dikonsumsi. Tujuan penelitian ini untuk mengetahui validitas metode QuEChERS dan GC-MS untuk analisis multi residu pestisida organoklorin dalam telur itik dan mendeteksi keberadaan multi residu organoklorin pada telur itik asal Kabupaten Bantul. Larutan standar yang digunakan terdiri dari campuran 17 jenis pestisida organoklorin. Telur itik diambil dari 138 peternakan itik yang berada di 10 kecamatan di Kabupaten Bantul. Telur itik diekstrak menggunakan kit QuEChERS extraction dan dibersihkan menggunakan kit QuEChERS dispersive SPE clean-up buah berlemak. Hasil pembersihan dianalisis menggunakan GC-MS, dengan pengaturan, suhu injektor 280 oC, suhu kolom 150-280 oC (suhu awal 150 oC (2,5 menit), dinaikkan 200 oC (3 menit) peningkatan suhu 8 oC/menit, suhu akhir 280 oC (3 menit) peningkatan suhu 6 oC/menit), suhu interface 280 oC, dan suhu ion source 300 oC. Berdasarkan data validasi yang diperoleh, metode analisis multi residu organoklorin pada telur itik menggunakan metode QuEChERS dan GC-MS pada penelitian ini valid dengan rekoveri antara 82% - 110% pada konsentrasi 0,05 mg/kg dan 0,1 mg/kg, limit deteksi (0,0003-0,0028 mg/kg) dan limit kuantitasi (0,001 - 0,0097 mg/kg) berada di bawah nilai batas maksimum residu yang ditetapkan SNI 01-6366-2000, presisi (RSD < 2/3 KVHorwitz), dan sensitivitas baik. Hasil pengujian multi residu pestisida organoklorin dalam telur itik diketahui residu 1,1-dichloro-2,2-bis (p-chlorophenyl) ethylene (DDE) terdeteksi pada 12 peternakan itik dengan konsentrasi antara 0,002 - 0,028 mg/kg. Dua dari 12 peternakan itik ini juga terdeteksi 1,1-dichloro-2,2-bis (p-chlorophenyl) ethane (DDD) dengan konsentrasi 0,008 mg/kg dan 0,01 mg/kg. Konsentrasi tersebut masih di bawah nilai BMR residu DDT dan metabolitnya sebesar 0,1 mg/kg.

Duck egg is source of animal protein that is an affordable food, however, it also suspected of having potential for contamination with some residues, such as organochlorin pesticide. The food safety assurance that suported by a valid testing laboratory have been necessary to ensure that food to be safe, of good quality, and suitable for consumption. The aim of this study are both to determine the validity of the QuEChERS method and chromatography gas-mass spectrometry (GC-MS) for analyzing multiresidues of organochlorine pesticide in duck eggs and to detect its in duck eggs from Bantul district. Duck eggs were colected from 138 duck farm samples located in 10 sub district. Standard solution were use mix of 17 analit of organochlorin pesticides. Duck eggs were extracted with QuECHERS extraction kit and cleaned up using dispersive SPE clean up kit for fatty fruits and then were analized by GC-MS with conditions were as follow, temperature of injector 280 oC, temperature of column was held at 150 oC for 2.5 min, then ramped to 200 oC for 3 min at 8 oC min-1, finally held at 280 oC for 3 min, temperature of interface at 280 oC, and temperature of ion source at 300 oC. Based on the validation data, the QuEChERS methods and GC-MS in this study is valid for testing organochlorin multiresidues in duck egg with recovery between 82% - 110% concentration at 0.05 mg/kg and 0.1 mg/kg, the limit of detection (0.0003 - 0.0028 mg/kg) and the limit of quantitation (0.001 - 0.0097 mg/ kg) were below the maximum residue limits specified by SNI 01-6366-2000, precision (RSD < 2/3 KVHorwitz), and has good sensitivity. Residue of 1,1-dichloro-2,2-bis p-chlorophenyl ethylene (DDE) in duck eggs were detected in 12 duck farms with a concentration between 0.002 - 0.028 mg/kg. Residue of 1,1-dichloro-2,2-bis (p-chlorophenyl) ethane (DDD) also were detected in two of these 12 duck farms with concentration are 0.008 mg/kg and 0.01 mg/kg. These concentration is still below the value of DDT and its metabolites residues of 0.1 mg/kg.

Kata Kunci : keamanan pangan, telur itik, multi residu organoklorin, metode QuEChERS, GC-MS, food safety, duck eggs, multi residues, organochlorin, QuEChERS methode, and GC-MS