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Contoh Soal

The document contains details on 6 sample analysis problems involving calculating theoretical and observed concentrations of active ingredients in pharmaceutical formulations based on spectroscopic data, and determining if the observed concentrations meet USP requirements. The problems involve analysis of amoxicillin tablets, paracetamol syrup, mefenamic acid and amoxicillin content in tablets using NIR spectroscopy, phenol content determination, and identification of phytochemicals using NIR spectroscopy. Calculations are shown to determine theoretical concentrations, observed concentrations from spectroscopic data, percentage recoveries, and whether results meet USP specifications.

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0% found this document useful (0 votes)
101 views4 pages

Contoh Soal

The document contains details on 6 sample analysis problems involving calculating theoretical and observed concentrations of active ingredients in pharmaceutical formulations based on spectroscopic data, and determining if the observed concentrations meet USP requirements. The problems involve analysis of amoxicillin tablets, paracetamol syrup, mefenamic acid and amoxicillin content in tablets using NIR spectroscopy, phenol content determination, and identification of phytochemicals using NIR spectroscopy. Calculations are shown to determine theoretical concentrations, observed concentrations from spectroscopic data, percentage recoveries, and whether results meet USP specifications.

Uploaded by

lintang
Copyright
© © All Rights Reserved
We take content rights seriously. If you suspect this is your content, claim it here.
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Soal Essay

1. Please read the data below and than answer the question :
 Label claim : each tablet consist of amoxicillin trihydrate equivalent to amoxicillin 500mg
 USP 25 requirement : Amoxicillin tablet contains not less than 90,0% and not more than 120,0% of
the labeled amount of amoxicillin
 Martindale 33th Ed : 1,15 g Amoxicillin trihydrate is approximately equivalent to 1 g of amoxicillin
 Sample preparation : Twenty tablets were weighed and their average weight was 650 mg. The
tablets were mixed and finely powdered. 35 mg of powdered sample was weighed and transferred into
a 100mL volumetric flask, and approximately 50 mL of the solvent was added. The mixture was
ultrasonicated for 5 min and then diluted to 100 mL with the same solvent. The solution was filtered
through a Whatman type-40 filter paper. The solution was observed by spectro UV Vis at 272 nm
 Result data from spectro UV Vis :
Identity Sample weight Concentration Absorbance
Standard solution 1 100 ppm 0.260
Standard solution 2 200 ppm 0.532
Standard solution 3 300 ppm 0.778
Standard solution 4 400 ppm 1.022
Sample X 35,0 mg 0.811
a. calculate the theoritical concentration of amoxicillin in the tablet %w/w ?
b. calculate the observation concentration of amoxicillin in the tablet %w/w ?
c. calculate % recovery of the sample? Does the concentration fulfilled the USP requirement?
Komposisi : tiap tablet (650mg) mengandung 500mg x 1,15 = 575mg amox trihidrat
Y = ...............x + ................
Y = 0,811  X= ......... ppm (µg/mL)  massa di labu 100mL = ........ µg/mL x 100mL = ....... µg =

%b/b = 1gram analit dalam 100gram sampel

%b/b =

%b/b teoritis =

%akurasi = kons hasil percon / kons teoritis x 100%

%akurasi =

2. Komposisi : Tiap 5mL mengandung parasetamol 120mg


Preparasi sample : dipipet 1,0 mL sample ditambah pelarut NaOH 0,01M ad 100,0mL, dikocok ad homogen,
dipipet 1,0mL ditambah NaOH 0,1 M ad 25 mL. Setelah diamati dengan spektrofotometer UV-Vis  257 nm
didapat data sbb:

Identitas Konsentrasi (ppm) Absorbasi


Standar 1 4,09 0,312
Standar 2 6,14 0,472
Standar 3 8,18 0,612
Standar 4 10,08 0,742
Standar 5 12,28 0,984
Sampel ?ppm ?mg 0,768

Hitung kadar bahan aktif dlm sirup Itramol %b/v dan %akurasi?
%b/v = 1 gram analit / 100mL sampel
Y = ...........x – ......................
Y = absorbansi
X = konsentrasi
Y =0,768  X= ..............ppm (µL/mL)massa dalam labu 25mL = .................................

Massa dalam labu 100mL  ....................................................................................... gram


%b/v =

% akurasi = konsentrasi hasil percobaan / kons teoritis x 100%

Kons teoritis  120mg/5mL = 0,120gram/5mL x 100% = 2,4%

% akurasi =

3. Preparasi sampel : 10 tablet amoksisilin ditimbang berat tabletnya, digerus, kemudian diayak dan dianalisis
dengan NIR. Data spektrum NIR dimasukkan kedalam model PLS dan didapat kadar asam mefenamat
dalam sampel sebesar 77,6%b/b. Bila berat tablet rata-rata 650,0 mg dan komposisi sampel tiap tablet
mengandung asam mefenamat 500 mg, apakah kadar sampel memenuhi persyaratan farmakope (90% -
110% dari label klaim).

4. Preparasi sampel : 10 tablet amoksisilin ditimbang berat tabletnya, digerus, kemudian diayak dan dianalisis
dengan NIR. Data spektrum NIR dimasukkan kedalam model PLS dan didapat kadar amoksisilin dalam
sampel sebesar 87,8%b/b. Bila berat tablet rata-rata 650,0 mg dan komposisi sampel tiap tablet mengandung
amoksisilin setara amoksisilin trihidrat 500 mg, apakah kadar sampel memenuhi persyaratan farmakope
(90% - 120% dari label klaim). Kesetaraan amoksisilin = 1,15 amoksisilin trihidrat.

5. Preparasi sample : ditimbang 20,0 mg sample ditambah pelarut ad 10,0mL, dikocok ad homogen, dipipet
200,0µL ditambah reagen folin dan Lar Na2CO3 ad 1,5mL. Setelah diamati dengan spektrofotometer UV-Vis
 628 nm didapat data kadar fenol 20,0ppm. Berapa kadar fenol dalam mg asam galat ekivalen per gram
sampel (mg AGE/g)
Massa dalam 1mL = 20,0 ppm = 20,0 µg/mL x 1 mL = 20,0 µg
Massa dalam 10,0mL = 20,0 µg x 10,0mL = 20,0 µg x 10.000µL = 2000,0µg = 2,0 mg AGE
100,0µL 100µL
Kadar fenol = 2,0 mg /20,0 mg sampel = 2,0 mg / 0,020gram sampel = 100,0 mg AGE/gram sampel

Massa dalam 1,5mL = 20,0 ppm = 20,0 µg/mL x 1,5 mL = 30,0 µg


Massa dalam 10,0mL = 30,0 µg x 10,0mL = 15,0 µg x 10.000µL = 1500,0µg = 1,5 mg AGE
200,0µL 100µL
Kadar fenol = 1,5 mg /20,0 mg sampel = 2,0 mg / 0,020gram sampel = 75,0 mg AGE/gram sampel

6. Untuk data NIR  yang terbaca pada model adalah konsentrasi 1/10 mg AGE/gram sampel
Kandunan fitokimia  fenol, flavonoid, alkalid, terpenoid, saponin tanin

1. Please read the data below and than answer the question :
 Label claim : each tablet consist of amoxicillin trihydrate equivalent to amoxicillin 500mg
 USP 25 requirement : Amoxicillin tablet contains not less than 90,0% and not more than 120,0% of
the labeled amount of amoxicillin
 Martindale 33th Ed : 1,15 g Amoxicillin trihydrate is approximately equivalent to 1 g of amoxicillin
 Sample preparation : Twenty tablets were weighed and their average weight was 650 mg. The
tablets were mixed and finely powdered. 35 mg of powdered sample was weighed and transferred into
a 100mL volumetric flask, and approximately 50 mL of the solvent was added. The mixture was
ultrasonicated for 5 min and then diluted to 100 mL with the same solvent. The solution was filtered
through a Whatman type-40 filter paper. The solution was observed by spectro UV Vis at 272 nm
 Result data from spectro UV Vis :
Identity Sample weight Concentration Absorbance
Standard solution 1 100 ppm 0.260
Standard solution 2 200 ppm 0.532
Standard solution 3 300 ppm 0.778
Standard solution 4 400 ppm 1.022
Sample X 35,0 mg 0.811
d. calculate the theoritical concentration of amoxicillin in the tablet %w/w ?
e. calculate the observation concentration of amoxicillin in the tablet %w/w ?
f. calculate % recovery of the sample? Does the concentration fulfilled the USP requirement?
Komposisi : tiap tablet (650mg) mengandung 500mg x 1,15 = 575mg amox trihidrat
Y = ...............x + ................
Y = 0,811  X= ......... ppm (µg/mL)  massa di labu 100mL = ........ µg/mL x 100mL = ....... µg =

%b/b = 1gram analit dalam 100gram sampel

%b/b =

%b/b teoritis =

%akurasi = kons hasil percon / kons teoritis x 100%

%akurasi =
 Label claim : each 5,0mL dry syrup consist of amoxicillin trihydrate equivalent to amoxicillin 120mg
Density of the syrup 1,12 g/mL  5,6gram syrup consist of amoxicillin trihydrate equivalent to
amoxicillin 120mg  5,6gram syrup consist of amoxicillin trihydrate 138mg
 USP 25 requirement : Amoxicillin tablet contains not less than 90,0% and not more than 120,0% of
the labeled amount of amoxicillin
 Martindale 33th Ed : 1,15 g Amoxicillin trihydrate is approximately equivalent to 1 g of amoxicillin
 Sample preparation : 1,22 g of syrup sample was weighed and transferred into a 100mL volumetric
flask, and approximately 50 mL of the solvent was added. The mixture was ultrasonicated for 5 min
and then diluted to 100 mL with the same solvent. The solution was filtered through a Whatman type-
40 filter paper. The solution was observed by spectro UV Vis at 272 nm
 Result data from spectro UV Vis :
Identity Sample weight Concentration Absorbance
Standard solution 1 100 ppm 0.260
Standard solution 2 200 ppm 0.532
Standard solution 3 300 ppm 0.778
Standard solution 4 400 ppm 1.022
Sample X
35,0 mg 0.811

g. calculate the theoritical concentration of amoxicillin in the tablet %w/w ?


h. calculate the observation concentration of amoxicillin in the tablet %w/w ?
i. calculate % recovery of the sample? Does the concentration fulfilled the USP requirement?

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