DAFTAR ISI
HALAMAN JUDUL ..................................................................................
i
HALAMAN PENGESAHAN .....................................................................
ii
HALAMAN MOTTO .................................................................................
iii
HALAMAN PERSEMBAHAN ..................................................................
iv
HALAMAN KATA PENGANTAR.............................................................
v
HALAMAN INTISARI ..............................................................................
vii
HALAMAN ABSTRACT ...........................................................................
viii
DAFTAR ISI ...............................................................................................
ix
DAFTAR GAMBAR ...................................................................................
xii
DAFTAR TABEL........................................................................................
xiv
DAFTAR LAMPIRAN ...............................................................................
xv
BAB I PENDAHULUAN 1.1.Latar Belakang........................................................................................
1
1.2. Rumusan Masalah ..................................................................................
4
1.3. Tujuan Penelitian ...................................................................................
4
1.4. Manfaat Penelitian .................................................................................
5
BAB II TINJAUAN PUSTAKA .................................................................
6
BAB III DASARTEORI .............................................................................
12
3.1.
Sensor ............................................................................................
12
3.1.1.
Sensor kimia ...................................................................................
13
3.2.
Elektro kimia ..................................................................................
14
3.3.
Voltametri Siklik .............................................................................
18
3.4.
Asam mefenamat .............................................................................
24
3.4.1
Farmakokinetika Asam Mefenamat .................................................
25
3.4.2.
Farmakodinamika Asam Mefenamat................................................
26
ix
3.4.3.
Efek Samping Asam Mefenamat......................................................
28
3.4.4.
Dosis Asam Mefenamat...................................................................
30
BAB IV METODE PENELITIAN 4.1.
AlatdanBahan..................................................................................
31
4.1.1.
Alat Penelitian.................................................................................
31
4.1.2.
Bahan Penelitian .............................................................................
31
4.2.
Cara Kerja.......................................................................................
32
4.2.1.
Pembuatan Larutan.........................................................................
32
4.2.2.
Preparasi Sampel.............................................................................
33
4.2.3.
Preparasi Instrumen........................................................................
33
4.2.4.
Karaktrisasi Puncak.........................................................................
34
4.2.5.
Analisis Variasi pH Buffer Fosfat ....................................................
34
4.2.6.
Analisis Variasi Elektrolit................................................................
35
4.2.7.
Analisis Variasi Scan rate................................................................
35
4.2.8.
Analisis Standar dan Sampel Asam Mefenamat ...............................
35
4.2.9.
Penentuan Nilai Presisi....................................................................
36
4.2.10. Penentuan Recovery Pengukuran.....................................................
36
4.2.11. Penentuan Limid Deteksi (LOD) dan limit kuantifikasi (LOQ)........
37
BAB V HASIL DAN PEMBAHASAN 5.1.
PenentuanPuncak ............................................................................
38
5.2.
Penentuan pH Optimum ..................................................................
39
5.3.
PenentuanElektrolit Optimum .........................................................
41
5.4.
Pengaruh Scan Rate.........................................................................
43
5.5.
PengaruhKonsentrasi.......................................................................
46
5.6.
AkurasiatauKecermatan ..................................................................
48
5.7.
Presisiatau Keseksamaan.................................................................
51
5.8.
Limit Deteksidan Limit Quantifikasi ...............................................
54
x
5.9.
Penentuankonsentrasisampel ...........................................................
56
BAB VI KESIMPULAN DAN SARAN 5.1.
Kesimpulan .....................................................................................
60
5.2.
Saran...............................................................................................
60
DAFTAR PUSTAKA ..................................................................................
59
LAMPIRAN ................................................................................................
61
xi
DAFTAR GAMBAR
Gambar 1.
Skema jalur kerja sensor.........................................................
12
Gambar 2.
Skema Sensor kimia...............................................................
14
Gambar 3.
Elektroda Nikel, Elektroda Platinum dan Elekroda Karbon (GCE) ....................................................................................
Gambar 4.
16
Elektroda kerja dan pembanding buatan sendiri yang berbentuk batang dan lempeng ...............................................
18
Gambar 5.
Contoh Voltamogram Siklik ...................................................
19
Gambar 6.
Voltamogram siklik scan dari potensial positif kearah potensialnegatif......................................................................
22
Gambar 7.
Struktur kimia asam mefenamat .............................................
23
Gambar 8.
Reaksi oksidasi asam mefenamat pada elektroda kerja ...........
23
Gambar 9.
Reaksi oksidasi asam mefenamat dengan oksigen ..................
24
Gambar 10.
Voltammogram hasil analisis puncak dengan menggunakan elektrolit buffer fosfat pH 4 dengan scan rate100 mV/s..........
Gambar 11.
Voltammogram pengaruh pH buffer fosfat terhadap arus dan puncak ...................................................................................
Gambar 12.
36 37
Penentuan elektrolit optimum dengan elektrolit KNO3 0,1 M, H2SO40,2 M dan buffer fosfat pH 4 pada analisis asam mefenamat 1000 ppm.............................................................
Gambar 13.
40
Pengaruhscan rate terhadap arus danpuncakvoltammogram pada potensial -1 sampai 1 volt ..............................................
42
Gambar 14.
Grafik kurva kalibrasi scan rate .............................................
43
Gambar 15.
Voltammogramhasilanalisisstandarasammefenamat
100-
1000ppm denganelektrolit buffer fosfat pH 4 pada scan rate 100 mV/s ............................................................................... Gambar 16.
Voltamogramhasilanalisissampel (merah)dansampel
yang
(biru),
mengandungstandar
44
standar (hijau)
menggunakan elektrolit buffer fosfat pH 4 pada scan rate100 mV/s ...................................................................................... xii
47
Gambar 17.
Voltammogram pengukuran arus sampel 10 kali pengulangan menggunakan scan rate 100 mv/s dengan waktu deposisi 5 detik.......................................................................................
50
Gambar 18.
Grafik hubungan antara konsentrasi (ppm) dengan arus (A) ...
53
Gambar 19.
Voltammogram hasil pengukuran standar asam mefenamat 100-1000 ppm dan tiga macam sampel asam mefenamat dengan menggunakan elektrolit buffer fosfat pH 4 pada scan
Gambar 20.
rate mV/s...............................................................................
55
Grafik hubungan antara konsentrasi (ppm) dengan arus (A) ...
56
xiii
DAFTAR TABEL
Tabel 1.
Hasil pengukuran arus asam mefenamat 1000 ppm pada variasi pH 2-7 dengan scan rate 100 mV/s .............................................
Tabel 2.
Hubungan antara variasi elektrolit dengan arus (A) pada voltammogram analisis asam mefenamat ....................................
Tabel 3.
Hubungan
antara
scan
rate
dengan
arus
(A)
40
pada
voltammogramanalisis asam mefenamat ..................................... Tabel 4.
38
42
Hasil pengukuran arus standar asam mefenamat konsentrasi 100-1000 ppm menggunakan elektrolit buffer fosfat pH 4pada scan rate 100 mV/s.....................................................................
Tabel 5.
44
Hasil pengukuran arus sampel, standar dan sampel yang mengandung standar menggunakan elektrolit buffer fosfat pH 4 pada scanrate 100 mV/s..............................................................
Tabel 6.
Hasil
pengukuran
arus
sampel
10
kali
pengulangan
menggunakan scanrate 100 mv/s dengan waktu deposisi 5 detik . Tabel 7.
47 50
Hasil pengukuran arus standar asam mefenamat 100-1000 ppm dengan menggunakan buffer fosfat pH 4 dengan scan rate 100 mV/S ...................................................................................
Tabel 8.
Hasil pengukuran arus tiga sampel obat menggunakan elektrolit Buffer fosfat pH 4 pada scan rate 100 mV/s ...............................
Tabel 9.
53 55
Hasil perhitungan % b/b masa sampel yang tertera dan massa sampel hasil analisis ...................................................................
xiv
56
DAFTAR LAMPIRAN
Lampiran 1.
Perhitunggan Presisi atau Keseksamaan .................................
62
Lampiran 2.
Perhitungan Recovery atau Akurasi ........................................
63
Lampiran 3.
Perhitunggan
Lampiran 4.
limit
of
detection
(LOD)
dan
Limit
ofQuantification (LOD)..........................................................
64
Perhitungan konsentrasi sampel..............................................
67
xv