2012_ review spektro uv-vis
TRANSCRIPT
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2UV-VIS 2012
SpektrofotometriSpektrofotometri
Teknik analisis yang berhubungan dengan
penggunaan cahaya untuk
- melihat pola spektrum senyawa- mengukur konsentrasi bahan
kimia
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3UV-VIS 2012
Alat apa yang digunakan ?
Spektrofotometer
Instrumen/AlatInstrumen/Alat
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4UV-VIS 2012
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5UV-VIS 2012
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Conventional Spectrophotometer
Optical system of a double-beam spectrophotometer
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7UV-VIS 2012
Radiasi ElektromagnetikRadiasi Elektromagnetik
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Energi Energi vs
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9UV-VIS 2012
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10UV-VIS 2012
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11UV-VIS 2012
SpektrofotometriSpektrofotometri
Ultraviolet:
: 190 - 400 nm
Visibel (sinar tampak):
: 400 - 700 nm
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12UV-VIS 2012
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13UV-VIS 2012
Spektrofotometri UVSpektrofotometri UV
Dasar analisis:- senyawa harus memiliki kromofor dan
auksokrom yang memadai
- kromofor adalah bagian molekul yang bertanggung jawab pada penyerapan cahaya
- auksokrom adalah gugus fungsi yang memiliki hetero atom dan menempel
langsung pada sistem kromofor
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14UV-VIS 2012
Spektrofotometri VisibelSpektrofotometri Visibel
Dasar analisis:- Senyawa asli/asal harus berwarna - Bila senyawa asli tidak berwarna,
dapat diubah menjadi senyawa berwarna dengan cara:
a. pembentukan senyawa komplekb. memperpanjang kromofor
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15UV-VIS 2012
Colors of Visible lightColors of Visible light
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16UV-VIS 2012
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17UV-VIS 2012
Penyerapan warna yang berbeda
Penyerapan warna yang berbeda
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UV-VIS 2012
Absorption of visible light
Where has the energy that was within the photons gone to ?
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Transmission and Color
The human eye sees the complementary color to that which is absorbed
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20UV-VIS 2012
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UV-VIS 2012
Lycophene [ dalam Tomat ]Lycophene [ dalam Tomat ]
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UV-VIS 2012
Zeaxanthin [ dalam Jagung ]
Zeaxanthin [ dalam Jagung ]
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UV-VIS 2012 23
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UV-VIS 2012
Senyawa berwarnaSenyawa berwarna
Karena
Senyawa Kompleks
24
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Kompleks logam berwarna dikarenakan:
Charge transfer transition
Perpindahan elektron (e-) dari: ion logam ke ligan
atau sebaliknya
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UV-VIS 2012
Senyawa kompleksSenyawa kompleks
Fe(CNS)3
Ferri salisilat
Protein-Biuret
ungu
ungu
merah darah
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Reaksi Biuret
ungu, 546 nm
NHO
NH
O
R
R
O
NH
O
R
R
Cu
peptidapeptida
NHNHO
NH
O
peptida
R
R
Cu2+
OH+2
ligan
ion logam
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Papaverin HClPapaverin HCl
N
CH2
OCH3
OCH3
H3CO
H3CO .HCl
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UV-VIS 2012
Kunang-kunang
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30UV-VIS 2012
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UV-VIS 2012 31
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32UV-VIS 2012
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UV-VIS 2012
Asam salisilatAsam salisilat
C
O
OH
H
O
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UV-VIS 2012
Absorpsi UV-VISAbsorpsi UV-VIS
akan mempromosikan (mentransisikan)
elektron
* (!)n *n * *
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36UV-VIS 2012
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Diagram Energi ElektronDiagram Energi Elektron
ENERGI
* [ anti ikatan ]
* [ anti ikatan ]
n [ tak terikat ]
[ ikatan ]
[ ikatan ]
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UV-VIS 2012
Transisi n π*Transisi n π*
Jenis transisi ini memiliki nilai ε kecil
Forbidden transition
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UV Excitation of 1,3-butadiene
1,3-butadiene
Transisi *
*
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Benzen kromoforBenzen kromofor
A1%1 cm
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Electronic TransitionElectronic Transition
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UV-VIS 2012
PustakaPustaka
Moffat, A.C., 1986, Clarke’s Isolation and iden- tification of drugs in pharmaceuticals,
body fluids, and post-mortem material, Second edition,
Pharmaceutical Press London.
Informasi Yang Diperoleh:- Kelarutan - Tes warna
- pKa - logP - Gas Chromatogr.- UV Spectrum - Infra Red Spectr.
- TLC - HPLC42
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PustakaPustaka
Galichet, L.Y., (Managing Editor), (2005) Clarke’s
Analysis of Drug and Poisons, Pharmaceu- tical Press, London.
Informasi Yang Diperoleh:- Kelarutan - Tes warna
- pKa - logP - Gas Chromatogr.- UV Spectrum - Infra Red Spectr.
- TLC - HPLC
UV-VIS 2012 43
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44UV-VIS 2012
SpektrofotometriSpektrofotometri
Analisis Kualitatif
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45UV-VIS 2012
FenobarbitalFenobarbital
C
H3C-H2CC
C
NH
NH
C O
O
O
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C
H3C-H2CC
C
NH
N
C O
O
O
_
Ultraviolet Spectrum
C
H3C-H2CC
C
NH
N
C O
O
O
_
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47UV-VIS 2012
Fenobarbital dalam larutan bufer pH 9,2
Fenobarbital dalam larutan bufer pH 9,2
C
H3C-H2CC
C
NH
N
C O
O
O
_
Kromofor
Auksokrom
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48UV-VIS 2012
Spektrum propil barbitalSpektrum propil barbital
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49UV-VIS 2012
Spektrum propil barbitalSpektrum propil barbitalSpektrum propil barbitalSpektrum propil barbital
C
H3C-H2CC
C
NH
NH
C O
O
O
Fenobarbital
Propil barbital
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UV-VIS 2012
Spektrum propil barbitalSpektrum propil barbitalSpektrum propil barbitalSpektrum propil barbital
C
H3C-H2CC
C
NH
NH
C O
O
O
Fenobarbital
Propil barbital
C
C
NH
NH
C O
O
O
H2C=CH-CH2
H2C=CH-CH2
C
239254
241256
max [ nm ]
50
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51UV-VIS 2012
Sulfadiazin
N
N
H2N S
O
O
NH
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N
N
H2N S
O
O
NH
H2N S
O
O
NH
N
N
CH3
N
N
H2N S
O
O
NH
CH3
CH3
Sulfadiazin
Sulfamerazin
Sulfamezatin
max [ nm ]
242254
242255
243258
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53UV-VIS 2012
Procain (dalam: asam, basa)Procain (dalam: asam, basa)
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54UV-VIS 2012
Phenylephrine (dalam: asam, basa)
Phenylephrine (dalam: asam, basa)
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55UV-VIS 2012
SpektrofotometriSpektrofotometri
Analisis Kuantitatif
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56UV-VIS 2012
Syarat Analisis Kuantitatif Secara Spektrofotometri
Suatu Zat
Syarat Analisis Kuantitatif Secara Spektrofotometri
Suatu Zat
Zat yang akan dianalisis harus memiliki kromofor yang mencukupi [ Amati dari nilai
koefisien ekstingsi Molar-nya ( ) harus lebih dari 1000 M-1.cm-1].
Larutan akhir sebelum diukur absorbannya harus jernih. Bila tidat jernih Terjadi penghamburan sinar oleh partikel yang tidak larut tersebut. Bgmn dengan nilai Abs. ?
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57UV-VIS 2012
Dasar Analisis Dasar Analisis KuantitatifKuantitatif
Dasar Analisis Dasar Analisis KuantitatifKuantitatif
Hukum Lambert-Beer
A = logTP
Plog 0
10
A = b c
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58UV-VIS 2012
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59UV-VIS 2012
Mana yang lebih disenangi
pembacaan Absorban atau Transmitan
Mana yang lebih disenangi
pembacaan Absorban atau Transmitan
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60UV-VIS 2012
Mengapa pembacaan Absorban tidak boleh lebih dari
satu
Mengapa pembacaan Absorban tidak boleh lebih dari
satu
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61UV-VIS 2012
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62UV-VIS 2012
Absorban vs indeks biasAbsorban vs indeks bias
22 2n
ncbεA
A = Absorbanε = koefisien ekstingsi molar (M-1.cm-1)
b = tebal larutan (kuvet) (cm)C = konsentrasi larutan (Molar, M)
n = indeks bias larutan
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UV-VIS 2012
The Magnitude of Molar absorptivity is 0 to around 105
= 0.87 x 1020 x P x a
P: transition probability (0 to 1) a: cross sectional target area in square centimeters (for organic molecules, this number is around 10-15 cm2).
Forbidden transition, P = 0.01; < 103
Allowed transition, P = 0.1 to 1 Weak absorption, = 103 L/ (mol*cm)Strong absorption, = 104 to 105 L/ (mol*cm)
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UV-VIS 2012
Untuk Analisis KuantitatifUntuk Analisis Kuantitatif
Senyawa yang
memiliki nilai koefisien ekstingsi molar [ ]
mudah dianalisis secara spektrofotommetri
≥ 1000 M -1. cm -1
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Rumus Pendekatan
Pada pelarut dan tertentu
1%1cmA
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Rumus Pendekatan
A = b c
= x 10
BM1%1cmA
= M-1. cm-1
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67UV-VIS 2012
PK. Ibuprofen, Spektro-UVPK. Ibuprofen, Spektro-UV
COOH
CH3
CH3
H3C
BM = 206,3
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68UV-VIS 2012
PK. Ibuprofen Spektro UV
PK. Ibuprofen Spektro UV
Pelarut ( 265
nm )
Air-basa 18,5
1%1cmA
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69UV-VIS 2012
PK. Clonidin, Spektro-UVPK. Clonidin, Spektro-UV
BM = 230,1
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70UV-VIS 2012
PK. Clonidin, Spektro-UVPK. Clonidin, Spektro-UV
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71UV-VIS 2012
PK. Difenilhidantoin, Spektro-UV
PK. Difenilhidantoin, Spektro-UV
NH
HN
O
O
BM = 252,3
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72UV-VIS 2012
PK. Difenilhidantoin Spektro UV
PK. Difenilhidantoin Spektro UV
Pelarut
Metanol
258 nm 264 nm
27 16
1%1cmA
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73UV-VIS 2012
PK. Clotrimazol, Spektro-UVPK. Clotrimazol, Spektro-UV
BM = 344,8BM = 344,8
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74UV-VIS 2012
PK. Clotrimazol, Spektro-UVPK. Clotrimazol, Spektro-UV
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75UV-VIS 2012
PK. Ampisilin, Spektro-UVPK. Ampisilin, Spektro-UV
BM = 349,4
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76UV-VIS 2012
PK. Ampisilin, Spektro-UVPK. Ampisilin, Spektro-UV
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77UV-VIS 2012
PK. Amoksisilin, Spektro-UVPK. Amoksisilin, Spektro-UV
BM = 365,4
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78UV-VIS 2012
PK. Amoksisilin, Spektro-UVPK. Amoksisilin, Spektro-UV
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79UV-VIS 2012
PK. Metampiron, Spektro-UVPK. Metampiron, Spektro-UV
NN
ON-CH2-SO3
CH3
CH3
CH3
Na+
BM = 351,4
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80UV-VIS 2012
PK. Metampiron Spektro UV
PK. Metampiron Spektro UV
Pelarut ( 258
nm )
Air-asam 266
1%1cmA
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81UV-VIS 2012
PK. Cortison, Spektro-UVPK. Cortison, Spektro-UV
BM = 360,4
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82UV-VIS 2012
PK. Cortison, Spektro-UVPK. Cortison, Spektro-UV
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83UV-VIS 2012
Apa Manfaat
Untuk Analisis Kuantitatif
???
Apa Manfaat
Untuk Analisis Kuantitatif
???
1%1cmA
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84UV-VIS 2012
SulfadiazinSulfadiazin
1%1cmA
Dalam etanol p.a, Sulfadiazin
memiliki
maks 270 nm dengan
Nilai = 8441%1cmA
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85UV-VIS 2012
Perkiraan Nilai AbsorbanPerkiraan Nilai Absorban
Berdasarkan Perhitungan Teorits Dari Nilai
dalam literatur
1%1cmA
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86UV-VIS 2012
Larutan induk Sulfadiazin 100 mg/100 mL (= 1 µg/µL)
Larutan induk Sulfadiazin 100 mg/100 mL (= 1 µg/µL)
Dipipet …. µL larutan induk, masukkan ke labu 25,0 mL. Tambahkan etanol ad 25,0 mL.
No. Li (µL) Tambahan etanol
(mL)
Kadar
(mg/25mL)
Absorban
teoritis
1 50 24,950 0,05 0,1692 100 24,900 0,10 0,3383 150 24,850 0,15 0,5064 200 24,800 0,20 0,6755 250 24,750 0,25 0,844
Y = b X + a r = …… ?
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87UV-VIS 2012
Nilai Absorban NyataNilai Absorban Nyata
Berdasarkan Hasil Pengukuran Pada Spektrofofometer
pada Nilai maks
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88UV-VIS 2012
Larutan induk Sulfadiazin 100 mg/100 mL (= 1 µg/µL)
Larutan induk Sulfadiazin 100 mg/100 mL (= 1 µg/µL)
Dipipet …. µL larutan induk, masukkan ke labu 25,0 mL. Tambahkan etanol ad 25,0 mL.
No. Li (µL) Tambahan etanol
(mL)
Kadar
(mg/25mL)
Absorban
nyata
1 50 24,95 0,05 0,1702 100 24,90 0,10 0,3373 150 24,85 0,15 0,5124 200 24,80 0,20 0,6795 250 24,75 0,25 0,850
Y = 3,404 X - 0,001 r = 0,9999
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89UV-VIS 2012
Setujukah Anda Dengan Teknik
Perhitungan Kadar
Obat
Tanpa Menggunakan
Standar
???
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UV-VIS 2012
CTMCTM
N CH(CH2)2N
Cl
CH3
CH3
OH
OH
H
H
O
O
.
90
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UV-VIS 2012
PK. CTM PK. CTM
Chinese Pharmacopoeia, Vol.II, 2005 [ p.185 ]Assay:
Measure the absorbance of the solution containing 20 g per mL in hydrochloric acid
solution ( 1 100 ) at 264 nm.Calculate the content of C16H19ClN2.C4H4O4,
taking 217 as the value of A ( 1%, 1 cm )
91
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UV-VIS 2012
CTMCTM
1%1cmA
Dalam larutan HCl ( 1 100 ), CTM memiliki
maks 264 nm dengan
Nilai = 2171%1cmA
92
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UV-VIS 2012
PK. Tablet AminofilinPK. Tablet AminofilinBritish Pharmacopoeia, Vol.III, 2007 [ p.2313 ]
Tablet Aminofilin:mengandung teofilin 80,6 – 90,8 % dan
etilendiamin tidak kurang dari 10,9 %.
Hitung kadar teofilin menggunakan nilai A 1% 1cm Teofilin dalam larutan NaOH 0,1 M pada 275 nm = 650.
Untuk Etilendiamin, ditetapkan secara titri-metri dengan larutan baku H2SO4 0,05 M, indi-kator larutan bromcresol green.
93
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94UV-VIS 2012
TeofilinTeofilin
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95UV-VIS 2012
Teofilin [ UV Spektrum ]Teofilin [ UV Spektrum ]
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96UV-VIS 2012
Moffat, A.C., 1986, [ Editor ] Clarke’s Isolation and Identification of Drugs
Second Edition, p.308
Moffat, A.C., 1986, [ Editor ] Clarke’s Isolation and Identification of Drugs
Second Edition, p.308
The divided into 3 category:Category 1:
The letter a after figure indicates that the value is a mean value based on several
reported figures all of which lie within a range of
+ 10% of the mean
1%1cmA
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97UV-VIS 2012
Moffat, A.C., 1986, [ Editor ] Clarke’s Isolation and Identification of Drugs
Second Edition, p.308
Moffat, A.C., 1986, [ Editor ] Clarke’s Isolation and Identification of Drugs
Second Edition, p.308
Category 2:
The letter b after a figure indicates that the value is a single reported value of
unknown reliability
1%1cmA
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98UV-VIS 2012
Moffat, A.C., 1986, [ Editor ]Clarke’s Isolation and Identification of Drugs
Second Edition, p.308
Moffat, A.C., 1986, [ Editor ]Clarke’s Isolation and Identification of Drugs
Second Edition, p.308
Category 3:
The letter c after a figure indicates that the value is a mean value based on
several reported figures some of which lie outside + 10%
of the mean
1%1cmA
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99UV-VIS 2012
Teknik Kuantifikasi AnalitMenggunakan
Standar
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100UV-VIS 2012
Plot Standar Untuk KuantitasiPlot Standar Untuk Kuantitasi
Dalam beberapa contoh di inndustri farmasi, produk obat dibuat dengan berbagai kadar, misal:
Tablet levotiroksin dengan kadar:
50, 100, 150, 200, 500, dan 750 g
Untuk keperluan mengembangkan dan memvalidasi metode
penetapan kadarnya, dapat ditempuh tiga strategi:
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101UV-VIS 2012
1. Single-Point Calibration1. Single-Point Calibration
Digunakan satu macam konsentrasi standarPlot stndar yang dibuat, digunakan untuk
menetapkan semua kadar tabletHal yang perlu diperhatikan adalah:
- metode ini perlu skema pengenceran dan ekstraksi yang berbeda untuk kadar obat yang bermacam-macam tersebut, dengan target:
Mendapatkan konsentrasi akhir serupa
Yang mendekati konsentarsi standar yang dibuat[ Respon Berdekatan ]
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Perbandingan AbsorbanPerbandingan Absorban
Absorban sampel
Absorban baku x Kadar baku = Kadar sampel
Syarat:
Nilai Abs.baku dan Nilai Abs.sampel
berdekatan
102Chan dkk., 2004, p.14.
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103UV-VIS 2012
2. Multiple-Point Calibration2. Multiple-Point Calibration
Digunakan seri konsentrasi standar yang dapat mengkover semua kadar produk obat tersebut.
Pda rentang konsentrasi tersebut, responnya harus linear.
Respon seluruh kadar obat (larutan akhir yang akan dibaca) berada pada rentang respon kurva kalibrasi.
Syarat:Tidak diperbolehkan adanya Ekstrapolasi
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105UV-VIS 2012
3. One Standard Calibration for Each Strength
3. One Standard Calibration for Each Strength
Digunaka satu konsentrasistandar untuk
setiap kadar obat
Kapan Metode ini dipilih ?
Apabila analit tidak menunjukkan linearitas pada rentang konsentrasi yang layak
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106UV-VIS 2012
Bagaimana Menghitung KadarBagaimana Menghitung Kadar
Denngan perbandingan nilai absorban sampel terhadap nilai absorban baku [yang sudah diketahui kadarnya]
Dengan menggunakan kurva baku/persamaan garis regresi linear.
Apa yang harus diperhatikan ?
Apa yang harus diperhatikan ?
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107UV-VIS 2012
Linearitas [ Menurut ICH, Q2(R1) ]Linearitas [ Menurut ICH, Q2(R1) ]
Linearitas suatu metode analisis:
adalah kemampuan metode tersebut (pada rentang tertentu)
untuk mencapai hasil uji yang berupa variasi data
(misal: absorban, luas area kromatogram) yang secara langsung proporsional terhadap
konsentrasi analit dalam sampel
Chan dkk., 2004, p.14.
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108UV-VIS 2012
Linearitas (lanjutan)Linearitas (lanjutan)
Variasi data yang dapat untuk meng-kuantifikasi analit dapat berupa:
- luas area kromatogram- tinggi puncak kromatogram- rasio antara luas area (tinggi puncak)
kromatogram analit terhadap luas area (tinggi puncak) kromatogram standar internal
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109UV-VIS 2012
Kuatitasi AnalitKuatitasi Analit
Tergantung pada kepatuhan pemenuhan hukum Beer
Tergantung linearitas pada rentang konsen-trasi tertentu
Oleh karenanya:- konsentrasi sampel kerja dan sampel
yang diuji untuk akurasi harus pada rentang yang linear
.
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110UV-VIS 2012
LinearitasLinearitas
Biasanya ditunjukkan langsung dengan pengenceran larutan baku stock.
Disarankan linearitas dikerjakan dengan seri pengenceran larutan stock.
Tidak disarankan mempersiapkan seri konsen-trasi larutan baku dengan seri penimbangan zat standar, karena:
Terjadi kesalahan penimbangan
Tidak menjamin diperolehnya linearitas yang baik
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111UV-VIS 2012
Evaluasi LinearitasEvaluasi Linearitas
Paling baik dilakukan dengan pengamatan secara visual plot respon (signal) sebagai fungsi konsentrasi analit.
Selanjutnya, variasi data umumnya digunakan untuk menghitung persamaan garis regresi dengan metode kuadrat terkecil ( Y = b X + a )
Syarat Linearitas:
Coeffcient of determination ( r2 ) ≥ 0.997
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112UV-VIS 2012
Rentang Linearitas [ ICH ]Rentang Linearitas [ ICH ]
Penetapan bahan obat atau produk obat:
± 20 % target atau konsentrasi nominal
Penetapan keragaman kandungan:
± 20 % target atau konsentrasi nominal
Pada rentang tersebut:
Paling tidak digunakan 5 (lima) macam tingkatan konsentrasi
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113UV-VIS 2012
Persamaan Garis RegresiPersamaan Garis Regresi
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116UV-VIS 2012
Bagaimana Cara
Mengalisis Campuran
Dua Senyawa
? ? ?
Bagaimana Cara
Mengalisis Campuran
Dua Senyawa
? ? ?
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117UV-VIS 2012
Two-Component MixtureTwo-Component Mixture
Example of a two-component mixture with little spectral overlap
X Y
X + Y
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118UV-VIS 2012
Two-Component MixtureTwo-Component Mixture
Example of a two-component mixture with significant spectral overlap
X
Y
X + Y
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125UV-VIS 2012