METODE PEMISAHAN

ANALISIS KIMIA FARMASI

Teknik pemisahan, pengukuran dan kesalahan analisis :
Teknik pemisahan dan pengukuran,
contoh-contoh reaksi aplikatif dalamanalisis farmasi

I NYOMAN KADJENG WIDJAJA

1. Pengendapan
2. Penguapan
1. Destilasi
2. sublimasi

3. Ekstraksi
1. Cair cair
2. Padat cair

4. Kromatografi
1. KLT
2. KG
3. KK

5. Elektroforesa
6. Penyaringan
7. Dll.

1. PENGENDAPAN
a. SUDAH TERBENTUK ; - campuran padat-cair
Dekantasi, Sentrifugasi
- Campuran padat-padat
magnetik, Eksklusi
b. DIBENTUK

: - campuran cair-cair
reaksi kimia
cair pada

2. PENGUAPAN
1. Campuran cair-cair
: - destilasi
2. Campuran padat-padat : - sublimas

3. EKSTRAKSI
1. EKTRAKSI CAIR-CAIR ( EEC/LLC)
2. EKSTRAKSI PADAT CAIR (EPC/SPE)
3. KROMATOGRAFI
1.
2.
3.
4.

KLT
KK
KG
K-EKSKLUSI

4. ELEKTROFORESA

KONSEP DASAR
EKSTRAKSI, KROMATOGRAFI

KOOFESIEN DISTRIBUSI
KOEFISIEN ADSORBSI
KOEFISIEN PARTISI

K , Kd, Kp

Kesalahan pada proses pemisahan

Pada penyaringan : pori pori saringan masih dapat
melewatkan lebih dari 1 ukuran komponen
Saat Penimbangan
Pada penguapan : titik didih atau titik penguapannya
berdekatan, - kebocoran pada saat penampungan
destilat
Saat pengukuran volume destilat
Ekstraksi/kromatografi, pemilihan sistem yg tidak cocok.
Kesalahan pada saat penyiapan sampel

Manfaat untuk dunia Farmasi

Memisahkan komponen aktif
Memurnikan bahan baku
Untuk pemekatan sampel analit

Tipe

Kegunaan

LC - 8

octyl bonded,
endcapped
silica

For reversed phase extraction of nonpolar to moderately polar

compounds, such as antibiotics, barbiturates,
benzodiazepines, caffeine, drugs, dyes, essential oils,
fat soluble vitamins, fungicides, herbicides, pesticides,
hydrocarbons, parabens, phenols,
phthalate esters, steroids, surfactants, theophylline, and water
soluble vitamins. Also
available in disk format.

ENVI-8

octyl bonded,
endcapped
silica

Higher phase coverage and carbon content than LC-8, greater

resistance to extreme pH conditions, and slightly higher
capacity for nonpolar compounds. For reversed phase
extraction of barbiturates, benzodiazepines, caffeine, drugs,
dyes, essential oils,
fat soluble vitamins, fungicides, herbicides, pesticides, PNAs,
hydrocarbons, parabens,
phenols, phthalate esters, steroids, surfactants, theophylline,
water soluble vitamins

LC - 4

butyldimethyl
bonded, endcapped silica
(500 pores)

Less hydrophobic than LC-8 or LC-18. For extraction of

peptides and proteins.

Tipe
LC - 18

octadecyl
bonded,
endcapped
silica

For reversed phase extraction of nonpolar to moderately polar

compounds, such as antibiotics, barbiturates, benzodiazepines,
caffeine, drugs, dyes, essential oils,
fat soluble vitamins, fungicides, herbicides, pesticides,
hydrocarbons, parabens, phenols,
phthalate esters, steroids, surfactants, theophylline, and water
soluble vitamins.

ENVITM18

octadecyl
bonded,
endcapped
silica

Higher phase coverage and carbon content than LC-18, greater

resistance to extreme pH conditions, and slightly higher capacity
for nonpolar compounds. For reversed phase
extraction of nonpolar to moderately polar compounds, such as
antibiotics, caffeine, drugs,
dyes, essential oils, fat soluble vitamins, fungicides, herbicides,
pesticides, PNAs,
hydrocarbons, parabens, phenols, phthalate esters, steroids,
surfactants, water soluble
vitamins.

Tipe

Kegunaan

LC-Ph

phenyl
bonded
silica

Slightly less retention than LC-18 or LC-8 material. For

reversed phase extraction of
nonpolar to moderately polar compounds, especially
aromatic compounds.

HisepTM

hydropho For exclusion of proteins in biological samples; retains

bic
small molecules such as drugs under reversed phase
surface
conditions
enclaved
by a
hydrophil
ic
network

LC-CN

cyanopro
pyl
bonded,
endcapp
ed silica

For reversed phase extraction of moderately polar

compounds, normal phase extraction of polar
compounds, such as aflatoxins, antibiotics, dyes,
herbicides, pesticides,
phenols, steroids. Weak cation exchange for
carbohydrates and cationic compounds

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