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REVIEW PRINSIP DASAR HPLC


Prinsip Kerja Fase diam Fase gerak Detektor Flow rate Struktur senyawa yang akan dianalisis

An-Sed-Far/Caroline/11
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Latihan Soal (1)

Metil Prednisolon

Prednisolon

Progesteron

Fase diam: ODS Fase Gerak : Metanol : Air = 60 : 40

An-Sed-Far/Caroline/11
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Latihan Soal (2)

Kodein

Morfin

Tebain

Fase diam: ODS Fase Gerak : Asetonitril : Dapar pH = 8.0 (10:90)

An-Sed-Far/Caroline/11
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REVIEW ANALISIS KUANTITATIF


Baku Internal vs Baku eksternal Isokratik vs Gradien Suhu kamar vs suhu tinggi Pasangan ion, penukar ion Derivatisasi

An-Sed-Far/Caroline/11
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PEMILIHAN METODE KROMATOGRAFI

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ION PAIR

Ion Pair Chromatography (IPC) is used to separate ionic analytes on a reversed phase column. An Ion Pair reagent is added to modulate retention of the ionic analytes. Typical IP reagents are:alkylsulphonates, alkylsulphates, tetra-alkylammonium ions etc.

An-Sed-Far/Caroline/11
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Efek Ion Pair

An-Sed-Far/Caroline/11
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Contoh Kasus pada KCKT

FG = Acetonitril : air = (5: 95) Famcyclovir, anti virus Herpes

FG = Acetonitril : air = (5: 95) , pH 2,5

FG = Acetonitril : sodium octylsulphonic acid 2 mM - KH2PO4 20 mM (5: 95), pH 2,5

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DERIVATISASI

Derivatization reagents may be divided into four groups:


- non-fluorescent reagents, generally used in UV-VIS - fluorogenic reagents, generally non-fluorescent but which react with target compounds to form conjugated fluorescent cyclic molecules (fluorescamine). - fluorescent reagents, which have a highly fluorescent aromatic group (fluophore) and a reactive group. -reagents with redox properties, used in electrochemistry. -Enantiomeric separation

An-Sed-Far/Caroline/11
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DERIVATISASI

Ninhidrin

O-phtalaldehyde + 2-merkaptoetanol

An-Sed-Far/Caroline/11
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Latihan Soal

Gabapentin, anti epilepsi

Adrenalin, hormon

Simvastatin, anti kolesterol

Riboflavin, vitamin

Naproxen, NSAIDs Glukosamine, obat artritis

An-Sed-Far/Caroline/11
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Latihan Soal
Pada suatu tablet yang mengandung Naproxen 100 mg dan Aspirin 250 mg pertablet, diketahui sbb: - Bobot 20 tablet = 10,3621 g - Bobot serbuk tablet yang ditentukan kadarnya = 257,1 mg yang dilarutkan dalam 250 ml pelarut kemudian diencerkan 200 kali pengenceran. - Kurva kalibrasi untuk Naproxen y = 174040x + 579, r = 0,999 - Kurva kalibrasi untuk Aspirin y = 54285 x + 1426, r = 0,999 x dalam satuan mg / 100 ml - Area yang diperoleh untuk sampel Naproxen adalah 72242 Area yang diperoleh untuk sampel Aspirin adalah 54819 Hitung kandungan Naproxen dan Aspirin !

An-Sed-Far/Caroline/11
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