Analisis kuantitatif sediaan obat multikomponen dengan spektrofluorometri
Preparasi untuk analisis sediaan obat multikomponen
Tahapan analisis kuantitatif obat kuantitatif obat multikomponen multikomponen dalam sediaan se diaan obat padat, semi padat, cair cair dan steril secara spektrofluorometri
M. SULAIMAN SULAIMAN ZUBAIR ZUBAIR (www.abuumar80.wordpress.com)
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Istilah y
y
y
Analisis
kuantitatif : analisis penentuan penentuan kadar suatu senyawa senyawa didalam suatu sampel Sediaan obat : padat (tablet, kapsul), semipadat (salep), cair (sirup, emulsi, suspensi) dan steril (injeksi) Multikomponen Multikomponen : sediaan obat yang terdiri dari beberapa be berapa senyawa senyawa aktif obat, seperti kombinasi GG dan Difenhidramin dalam sirup obat batuk
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Preparasi
sediaan obat multik multikomponen omponen untuk analisis kuantitatif dengan spektrofluor spektrofluorometri ometri -
Sampel tablet yang akan dianalisis harus representatif untuk menghindari resiko adanya hasil analisis yang keluar dari spesifikasi yang ditentukan. Contoh : Menurut Farmakope, untuk analisis tablet parasetamol dibutuhkan sampel sebanyak sebanyak 20 tablet parasetamol 500 mg
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Preparasi
sediaan obat multik multikomponen omponen untuk analisis kuantitatif dengan spektrofluor spektrofluorometri ometri y
y
Sediaan cair : dapat dilakukan pengukuran secara langsung, atau diencerkan atau dipekatkan dipekatkan terlebih dahulu dengan pelarut pelar ut organik Sediaan steril (injeksi) : dapat dilakukan pengukuran secara langsung
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Preparasi
sediaan obat multik multikomponen omponen untuk analisis kuantitatif dengan spektrofluor spektrofluorometri ometri Sediaan semi padat Isolasi obat dalam salep harus ditunjukkan ditunjukkan pada dasar salepnya : - Salep lemak bulu domba alkohol, biasanya dilarutkan dalam kloroform atau eter - Salep hidrofil, dilarutkan dalam kloroform atau eter - Salep lanolin, dilarutkan dalam kloroform atau eter Salep Polietilen glikol, dilarutkan dalam etanol atau air y
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y
y
Pada prinsipnya, semua pengukuran dengan menggunakan menggunakan instrumen instr umen spektroskopi, spektroskopi, maka maka syarat pertama pertama adalah harus larut dalam larutan pembawa yang digunakan Meskipun sediaan itu merupakan sediaan obat multikomponen, maka dengan instrumen spektroskopi spektroskopi maupun kromatografi kromatografi dapat membedakan masingmasing komponen tersebut, berdasarkan
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Tinjauan y
Umum Spektrofluorometri
Spektrofotometri fluoresensi merupakan suatu prosedur yang menggunakan pengukuran intensitas cahaya cahaya fluoresensi yang dipancarkan oleh zat uji dibandingkan
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Instrumentasi y
Pengukuran intensitas fluoresensi dapat dilakukan dengan suatu fluorometer filter
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Fluoresensi y
dan Struktur Molekul
Supaya terjadi fluoresensi, harus terjadi peresapan cahaya yang kuat oleh suatu molekul. Hal ini dapat terjadi ter jadi pada s wa aromati
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Tabel dari beberapa senyawa yang dapat
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Dengan suatu pereaksi tertentu, senyawa yang tidak
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Hubungan
Struktur Molekul dan
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kelompok analisis obat secara
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kelompok analisis obat secara
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b. Pengolahan engolahan Data Pengenceran Larut Larutan an awal wal : 100 100 ppm ppm 1. Dib Dibuat uat Larut Larutan an St Stok ok : 1 ppm Perhitungan V1.M1 = V2.M2 V1.1 V1 .100 00 ppm ppm = 100 100 mL. mL. 1ppm 1ppm V1 = 1 mL 2. Larutan Larutan stand standar ar : 0,1 ppm ppm V1.M1 = V2.M2 V1.1 V1 .1 ppm ppm = 25 mL 0,1p 0,1ppm pm
4. Laru Laruta tan n
stan standa darr :
0,2 ppm V1.M1 = V2.M2 V1.1 V1 .1 ppm ppm = 25 mL. mL. 0,2ppm V1 = 5 mL 5. Laru Laruta tan n St Stan and dar : 0,25 ppm V1.M1 = V2.M2 V1.1 V1 .1 ppm ppm = 25 mL. mL. 0,25ppm V1 = 6,25 mL 6. Laru Laruta tan n St Stan and dar : 0,3 ppm
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y
Tabel 2. Pengolahan Data Bahan
Intensita Inte nsitass pada =450 nm
Intensita Inte nsitass BahanBahan-Blank Blanko o pada =450nm
Blanko
0,4
-
Sampel
31
30,6
0,1 ppm
14
13,6
0,15 ppm
19.9
19,5
0,2 ppm
26
25,6
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y
Dari grafik didapatkan persamaan regresi: y = bx + a I = m.C + Io I = 124,2 C + 0,94 Dengan perhitungan kalkulator didapat R2 = 1 Maka dapat diketahui konsentrasi sampel dengan cara substitusi nilai intensitas sampel dikurangi blanko pada panjang gelombang ge lombang 450nm. I sampel = 30,6 I = 124,2 C + 0,94 I = 124,2 C + 0,94 C = 0,23 ppm
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Sekian dan Terimakasih WASSALAM