s kim 0800652 table of content
v
DAFTAR ISI
ABSTRAK ...................................................................................................... i
KATA PENGANTAR .................................................................................... ii
DAFTAR ISI ................................................................................................... v
DAFTAR TABEL........................................................................................... viii
DAFTAR GAMBAR ...................................................................................... ix
DAFTAR LAMPIRAN .................................................................................. x
BAB I PENDAHULUAN ............................................................................... 1
1.1 Latar Belakang................................................................................. 1
1.2 Rumusan Masalah............................................................................ 4
1.3 Batasan Masalah .............................................................................. 4
1.4 Tujuan Penelitian ............................................................................. 4
1.5 Manfaat Penelitian ........................................................................... 5
BAB II TINJAUAN PUSTAKA .................................................................. 6
2.1 Validasi Metode .............................................................................. 6
2.1.1
Linearitas ............................................................................ 7
2.1.2
Batas deteksi atau Limit of Detection (LOD) ..................... 8
2.1.3
Batas kuantitasi atau Limit of Quantitation (LOQ) ............ 8
2.1.4
Presisi ................................................................................. 9
2.1.5
Akurasi (Kecermatan) ........................................................ 10
2.1.6
Spesifitas ............................................................................ 11
2.1.7
Kisaran (Range) ................................................................. 11
Dian Novita Zebua, 2013
Validasi Metode Dan Penentuan Cemaran Melamin Dalam Susu Formula Menggunakan High
Performance Liquid Chromatography Hitachi D 7000
Universitas Pendidikan Indonesia | repository.upi.edu
vi
2.1.8
Ketahanan (Robustness) ..................................................... 11
2.1.9
Ketangguhan Metode (ruggedness) ................................... 12
2.1.10 Kesesuaian Sistem.............................................................. 12
2.2 Melamin ........................................................................................... 13
2.2.1
Produksi dan Penguraian Melamin .................................... 15
2.2.2
Kontaminasi Melamin ........................................................ 16
2.2.3
Analisis Melamin ............................................................... 19
2.3 Susu Formula ................................................................................... 20
2.4 High Performance Liquid Chromatography (HPLC) ..................... 22
2.4.1
HPLC Fase Terbalik atau Reverse Phase HPLC
(RP-HPLC) ......................................................................... 23
2.4.2
Instrumentasi HPLC ........................................................... 26
2.5 Trifluoroacetic Acid (TFA) ............................................................. 28
BAB III METODE PENELITIAN .................................................................. 30
3.1 Lokasi Penelitian ............................................................................. 30
3.2 Alat dan Bahan ................................................................................ 30
3.2.1
Alat ..................................................................................... 30
3.2.2
Bahan.................................................................................. 30
3.3 Metode Penelitian ............................................................................ 31
3.3.1
Preparasi ............................................................................. 32
3.3.2
Penentuan Kondisi Analisis ............................................... 35
3.3.3
Validasi Metode ................................................................. 36
Dian Novita Zebua, 2013
Validasi Metode Dan Penentuan Cemaran Melamin Dalam Susu Formula Menggunakan High
Performance Liquid Chromatography Hitachi D 7000
Universitas Pendidikan Indonesia | repository.upi.edu
vii
BAB IV HASIL PENELITIAN DAN PEMBAHASAN ................................. 39
4.1 Penentuan Kondisi Analisis ............................................................. 39
4.1.1
Penentuan pH fase gerak TFA 0,1% .................................. 39
4.1.2
Penentuan komposisi fase gerak ........................................ 40
4.1.3
Penentuan laju alir .............................................................. 41
4.2 Validasi Metode ............................................................................... 42
4.2.1
Penentuan linearitas ........................................................... 42
4.2.2
Batas deteksi atau limit of detection (LOD) ....................... 44
4.2.3
Batas kuantisasi atau limit of kuantitation (LOQ).............. 45
4.2.4
Penentuan presisi (keterulangan) ....................................... 45
4.2.5
Akurasi ............................................................................... 46
BAB V KESIMPULAN DAN SARAN ............................................................ 49
5.1
Kesimpulan ................................................................................. 49
5.2
Saran............................................................................................ 49
DAFTAR PUSTAKA ........................................................................................ 50
LAMPIRAN-LAMPIRAN ............................................................................... 53
Dian Novita Zebua, 2013
Validasi Metode Dan Penentuan Cemaran Melamin Dalam Susu Formula Menggunakan High
Performance Liquid Chromatography Hitachi D 7000
Universitas Pendidikan Indonesia | repository.upi.edu
DAFTAR ISI
ABSTRAK ...................................................................................................... i
KATA PENGANTAR .................................................................................... ii
DAFTAR ISI ................................................................................................... v
DAFTAR TABEL........................................................................................... viii
DAFTAR GAMBAR ...................................................................................... ix
DAFTAR LAMPIRAN .................................................................................. x
BAB I PENDAHULUAN ............................................................................... 1
1.1 Latar Belakang................................................................................. 1
1.2 Rumusan Masalah............................................................................ 4
1.3 Batasan Masalah .............................................................................. 4
1.4 Tujuan Penelitian ............................................................................. 4
1.5 Manfaat Penelitian ........................................................................... 5
BAB II TINJAUAN PUSTAKA .................................................................. 6
2.1 Validasi Metode .............................................................................. 6
2.1.1
Linearitas ............................................................................ 7
2.1.2
Batas deteksi atau Limit of Detection (LOD) ..................... 8
2.1.3
Batas kuantitasi atau Limit of Quantitation (LOQ) ............ 8
2.1.4
Presisi ................................................................................. 9
2.1.5
Akurasi (Kecermatan) ........................................................ 10
2.1.6
Spesifitas ............................................................................ 11
2.1.7
Kisaran (Range) ................................................................. 11
Dian Novita Zebua, 2013
Validasi Metode Dan Penentuan Cemaran Melamin Dalam Susu Formula Menggunakan High
Performance Liquid Chromatography Hitachi D 7000
Universitas Pendidikan Indonesia | repository.upi.edu
vi
2.1.8
Ketahanan (Robustness) ..................................................... 11
2.1.9
Ketangguhan Metode (ruggedness) ................................... 12
2.1.10 Kesesuaian Sistem.............................................................. 12
2.2 Melamin ........................................................................................... 13
2.2.1
Produksi dan Penguraian Melamin .................................... 15
2.2.2
Kontaminasi Melamin ........................................................ 16
2.2.3
Analisis Melamin ............................................................... 19
2.3 Susu Formula ................................................................................... 20
2.4 High Performance Liquid Chromatography (HPLC) ..................... 22
2.4.1
HPLC Fase Terbalik atau Reverse Phase HPLC
(RP-HPLC) ......................................................................... 23
2.4.2
Instrumentasi HPLC ........................................................... 26
2.5 Trifluoroacetic Acid (TFA) ............................................................. 28
BAB III METODE PENELITIAN .................................................................. 30
3.1 Lokasi Penelitian ............................................................................. 30
3.2 Alat dan Bahan ................................................................................ 30
3.2.1
Alat ..................................................................................... 30
3.2.2
Bahan.................................................................................. 30
3.3 Metode Penelitian ............................................................................ 31
3.3.1
Preparasi ............................................................................. 32
3.3.2
Penentuan Kondisi Analisis ............................................... 35
3.3.3
Validasi Metode ................................................................. 36
Dian Novita Zebua, 2013
Validasi Metode Dan Penentuan Cemaran Melamin Dalam Susu Formula Menggunakan High
Performance Liquid Chromatography Hitachi D 7000
Universitas Pendidikan Indonesia | repository.upi.edu
vii
BAB IV HASIL PENELITIAN DAN PEMBAHASAN ................................. 39
4.1 Penentuan Kondisi Analisis ............................................................. 39
4.1.1
Penentuan pH fase gerak TFA 0,1% .................................. 39
4.1.2
Penentuan komposisi fase gerak ........................................ 40
4.1.3
Penentuan laju alir .............................................................. 41
4.2 Validasi Metode ............................................................................... 42
4.2.1
Penentuan linearitas ........................................................... 42
4.2.2
Batas deteksi atau limit of detection (LOD) ....................... 44
4.2.3
Batas kuantisasi atau limit of kuantitation (LOQ).............. 45
4.2.4
Penentuan presisi (keterulangan) ....................................... 45
4.2.5
Akurasi ............................................................................... 46
BAB V KESIMPULAN DAN SARAN ............................................................ 49
5.1
Kesimpulan ................................................................................. 49
5.2
Saran............................................................................................ 49
DAFTAR PUSTAKA ........................................................................................ 50
LAMPIRAN-LAMPIRAN ............................................................................... 53
Dian Novita Zebua, 2013
Validasi Metode Dan Penentuan Cemaran Melamin Dalam Susu Formula Menggunakan High
Performance Liquid Chromatography Hitachi D 7000
Universitas Pendidikan Indonesia | repository.upi.edu