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A good linear relationship (r = 0.998) was observed between

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yahya pacha

on 14 April 2014

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Transcript of A good linear relationship (r = 0.998) was observed between

Spectroscopic Determination of Ibandronic Acid
A good linear relationship (r = 0.998) was observed between the concentration range of linearity in the range of 25-150 μg/mL for Ibandronic Acid respectively.


The absence of additional peaks in the chromatogram indicated noninterference of the common excipients used in the tablets.


Satisfactory separation and good peak shapes were achieved with a flow rate of 0.8 ml min-1.




Table for Standard Calibration Values of Ibandronic Acid

The mobile phase consists of Buffer: ACN (50:50 v/v); Flow rate 0.8ml min−1 at ambient temperature.

The analytes were monitored by UV detector. The injection volume was 20 μL with a flow rate 0.8 mL min-1 and detection Wavelength 272 nm having ambient condition and run time 7 min.

The method was validated for specificity, precision, linearity, and accuracy.


The average recoveries for Ibandronic Acid were in the range of 99.0–102.0% and the method can be successfully applied for the routine analysis of the drug substance.


The HPLC procedures in the Assay, Limit of Ibandronate Related in Compound A test, and test for Limit of Phosphate and Phosphite are based on analyses performed with the Allsep Anion brand of phase L23 column.

The typical retention times for the ibandronate peak in the Assay and Limit of Ibandronate Related Compound A tests are about 9–11 min.

In the test for Limit of Phosphate and Phosphite, about 12.5 min. The typical retention time for formic acid is 5.4 min.

under USP‘s Pending Monographs Guideline 2010 The United States Pharmacopeia.
http://www.usp.org


Calculate the percentage of ibandronate sodium (C9H22NNaO7P2) in the portion of Ibandronate Sodium taken:
Result = (rU/rS) ´ (CS/CU) ´ 100

rU = peak response of ibandronate in the Sample solution
rS = peak response of ibandronate in the Standard solution
CS = concentration of USP Ibandronate Sodium RS in
the Standard solution (mg/mL)
CU = concentration of Ibandronate Sodium in the Sample
solution (mg/mL)

Acceptance criteria: 98.0%–102.0% on the dried basis


The flow rate was 1.0 mL/min.

The relative standard deviation of peak area was 0.8%.

The linear correlation was observed from 300 mg/L -1,500 mg/L of Ibandronate (r = 0.9989).

The lowest detectable concentration of Ibandronate was 6 mg/L.

The method is simple, rapid and reproducible


Ibandronic acid may be used to treat high levels of calcium in the blood (hypercalcaemia) caused by secondary bone cancer.

Ibandronic acid (INN) or ibandronate sodium (USAN), marketed under the trade names Boniva® in the USA, Bondronat® in Europe, Bonviva® in Asia, and ADRONiL by Searle in Pakistan.





Presented to Prof. Mohie Sharaf El-Din


Prepared By:

Amir Elgendy Amir Hadaya Nada Hamouda

Conclusion:


Statistical analysis proves that the method is repeatable, selective and accurate for the determination of investigated drug.


A mixture of 2.5 gms of Sodium Lauryl Sulphate in 1000 ml of 0.1N Potassium Di Hydrogen Phosphate with Acetonitrile (50:50 v/v) was found to be the most suitable solvent for elution to obtain well defined peaks, free from tailing as per the ICH guidelines.


In the HPLC method, the standard and sample preparations required less time and no tedious extraction were involved thereof.



RESULTS AND DISCUSSION


The proposed RP-HPLC method for the estimation of Ibandronic Acid in tablet dosage forms is accurate, precise, linear, robust, simple and rapid.
Hence the present RP-HPLC method is suitable for the quality control of the raw material, formulation and dissolution studies.
From the typical chromatogram of Ibandronic Acid ,the retention time was found to be 3.608 minutes.


Figure 2. Typical chromatogram of working standard sample of Ibandronic Acid
 


Figure 1. Typical chromatogram of standard Ibandronic Acid




A simple, accurate and sensitive liquid chromatographic method has been developed for the determination of Ibandronic Acid (IBN) in tablet dosage form.

The separation was achieved using analytical column Inertsil ODS C18, 250 X 4.6 mm, 5 μm.

International Journal of Pharma Sciences Vol. 4, No. 1 (2014): 442-446






Analytical Method Development and Validation of Ibandronic Acid in API and Its Tablet Dosage Form by LC
( Reverse Phase HPLC)


Ibandronate Sod. Method of Analysis

Assay: Procedure:

Mobile phase: Add 2.0 mL of formic acid to 1 L of water and adjust the pH of the solution to 3.3 with ammonia solution.

Standard solution: 2 mg/mL of USP Ibandronate Sodium RS in Mobile phase

Sample solution: 2 mg/mL of Ibandronate Sodium in Mobile phase.

Chromatographic System:
Mode: LC Detector: Refractive index Detector

Temperature: 35° Column: 4.6-mm ´ 15-cm; 7-mm packing L23

Column temperature: 60° Flow rate: 0.5–0.7 mL/min

Injection size: 50 mL


Ibandronate sodium has the following structural formula:




Preparations: Tablets: 150 mg; Intravenous injection, 3 mg/3 ml.

BONIVA (ibandronate sodium) is a nitrogen-containing bisphosphonate.

The chemical name for ibandronate sodium is 3-(N-methyl-N-pentyl) amino-1-hydroxypropane-1,1diphosphonic acid, monosodium salt, monohydrate.

The molecular formula C9H22NO7P2Na•H2O with a molecular weight of 359.24.

Ibandronate sodium is a white- to off-white powder.
It is freely soluble in water and practically insoluble in organic solvents

Ibandronic Acid

Ibandronate is a potent bisphosphonate drug used in the prevention and treatment of osteoporosis.

Used to prevent bone problems in people whose cancer has weakened the bone. It is most commonly used to treat breast cancer that has spread to the bone (secondary breast cancer).



What ibandronic acid is?

Ibandronate can form a complex compound with the copper ion added in the mobile phase.

The complex can be detected at UV 240 nm.

The effects of pH of mobile phase and concentration of methanol to the retention time were studied.

Concentration of 10% methanol and pH 2.5 were suitable for the detection in less than 5 min.


Determination of ibandronate by high performance ion exchange chromatography

A good linear relationship
(r = 0.998)
was observed between the concentration range of linearity in the range of
25-150 μg/mL
for Ibandronic Acid respectively.

The absence of additional peaks in the chromatogram indicated noninterference of the common excipients used in the tablets.

Satisfactory separation and good peak shapes were achieved with
a flow rate of 0.8 ml min-1.




A mixture of 2.5 gms of Sodium Lauryl Sulphate in 1000 ml of 0.1N Potassium Di Hydrogen Phosphate with Acetonitrile (50:50 v/v) was found to be the most suitable solvent for elution to obtain well defined peaks, free from tailing as per the ICH guidelines.


In the HPLC method, the standard and sample preparations required less time and no tedious extraction were involved thereof.



Table for Standard Calibration Values of Ibandronic Acid

The mobile phase consists of Buffer:
ACN (50:50 v/v); Flow rate 0.8ml min−1 at ambient temperature.

The analytes
were monitored by UV detector. The injection volume was 20 μL with a flow rate 0.8 mL min-1 and detection Wavelength 272 nm having ambient condition and run time 7 min.

The method was validated for specificity, precision, linearity, and accuracy.

The average recoveries for Ibandronic Acid were in the range of
99.0–102.0%
and the method can be successfully applied for the routine analysis of the drug substance.


The
HPLC
procedures in the Assay, Limit of Ibandronate Related in Compound A test, and test for Limit of
Phosphate and Phosphite
are based on analyses performed with the Allsep Anion brand of phase L23 column.

The typical retention times for the ibandronate peak in the Assay and Limit of Ibandronate Related Compound A tests are about
9–11 min
.

In the test for Limit of Phosphate and Phosphite, about
12.5 min
. The typical retention time for formic acid is
5.4 min
.

under USP‘s Pending Monographs Guideline 2010 The United States Pharmacopeia. http://www.usp.org


Calculate the percentage of ibandronate sodium (
C9H22NNaO7P2
) in the portion of Ibandronate Sodium taken:

Result = (rU/rS) ´ (CS/CU) ´ 100

rU =
peak response of ibandronate in the Sample solution
rS =
peak response of ibandronate in the Standard solution
CS =
concentration of USP Ibandronate Sodium RS in
the Standard solution (mg/mL)
CU =
concentration of Ibandronate Sodium in the Sample
solution (mg/mL)

Acceptance criteria: 98.0%–102.0% on the dried basis


The flow rate was
1.0 mL/min
.

The relative standard deviation of peak area was
0.8%
.

The linear correlation was observed from
300 mg/L -1,500 mg/L
of Ibandronate

(r = 0.9989).

The lowest detectable concentration of Ibandronate was
6 mg/L.

The method is simple, rapid and reproducible


Preparations: Tablets: 150 mg; Intravenous injection, 3 mg/3 ml.

BONIVA (ibandronate sodium) is a nitrogen-containing bisphosphonate.

The chemical name for ibandronate sodium is 3-(N-methyl-N-pentyl) amino-1-hydroxypropane-1,1diphosphonic acid, monosodium salt, monohydrate.

The molecular formula C9H22NO7P2Na•H2O with a molecular weight of 359.24.

Ibandronate sodium is a white- to off-white powder.
It is freely soluble in water and practically insoluble in organic solvents

Ibandronic Acid

Ibandronic acid may be used to treat high levels of calcium in the blood (hypercalcaemia) caused by secondary bone cancer.

Ibandronic acid (INN) or ibandronate sodium (USAN), marketed under the trade names Boniva® in the USA, Bondronat® in Europe, Bonviva® in Asia, and ADRONiL by Searle in Pakistan.





Presented to Prof. Mohie Sharaf El-Din


Prepared By:

Amir Elgendy Amir Hadaya Nada Hamouda

Conclusion:


Statistical analysis proves that the method is repeatable, selective and accurate for the determination of investigated drug.


RESULTS AND DISCUSSION


The proposed RP-HPLC method for the estimation of Ibandronic Acid in tablet dosage forms is accurate, precise, linear, robust, simple and rapid.

Hence the present
RP-HPLC
method is suitable for the quality control of the raw material, formulation and dissolution studies.
From the typical chromatogram of Ibandronic Acid ,the retention time was found to be

3.608 minutes
.


Figure 2. Typical chromatogram of working standard sample of Ibandronic Acid
 


Figure 1. Typical chromatogram of standard Ibandronic Acid




A simple, accurate and sensitive liquid chromatographic method has been developed for the determination of Ibandronic Acid (IBN) in tablet dosage form.

The separation was achieved using analytical column Inertsil ODS C18, 250 X 4.6 mm, 5 μm.








Analytical Method Development and Validation of Ibandronic Acid in API and Its Tablet Dosage Form by LC
(
Reverse Phase HPLC
)


Ibandronate Sod. Method of Analysis

Assay: Procedure:

Mobile phase: Add 2.0 mL of formic acid to 1 L of water and adjust the pH of the solution to 3.3 with ammonia solution.

Standard solution: 2 mg/mL of USP Ibandronate Sodium RS in Mobile phase

Sample solution: 2 mg/mL of Ibandronate Sodium in Mobile phase.

Chromatographic System:
Mode: LC Detector: Refractive index Detector

Temperature: 35° Column: 4.6-mm ´ 15-cm; 7-mm packing L23

Column temperature: 60° Flow rate: 0.5–0.7 mL/min

Injection size: 50 mL


Ibandronate can form a complex compound with the
copper ion
added in the mobile phase.

The complex can be detected at
UV 240 nm
.

The effects of pH of mobile phase and concentration of methanol to the retention time were studied.

Concentration of
10% methanol
and pH
2.5
were suitable for the detection in less than 5 min.


Determination of ibandronate by high performance ion exchange chromatography

Ibandronate sodium has the following structural formula:




Ibandronate is a potent bisphosphonate drug used in the prevention and treatment of osteoporosis.

Used to prevent bone problems in people whose cancer has weakened the bone. It is most commonly used to treat breast cancer that has spread to the bone (secondary breast cancer).



What ibandronic acid is?


Presented to Prof.Dr: Mohie Sharaf El-Din


Prepared By:
Amir Elgendy Amir Hadaya Nada Hamouda
What ibandronic acid is?
Ibandronate is a potent bisphosphonate drug used in the prevention and treatment of osteoporosis.

Used to prevent bone problems in people whose cancer has weakened the bone. It is most commonly used to treat breast cancer that has spread to the bone (secondary breast cancer).

Ibandronic acid may be used to treat
high levels of calcium
in the blood (hypercalcaemia) caused by
secondary bone cancer.

Ibandronic acid (INN) or ibandronate sodium (USAN), marketed under the trade names
Boniva®
in the USA,
Bondronat®
in Europe,
Bonviva®
in Asia, and
ADRONiL
by Searle in Pakistan.

Ibandronic Acid
Preparations:
Tablets: 150 mg; Intravenous injection, 3 mg/3 ml.

BONIVA (ibandronate sodium) is a nitrogen-containing bisphosphonate.

The chemical name for ibandronate sodium is 3-(N-methyl-N-pentyl)
amino
-1-hydroxypropane-1,1
diphosphonic
acid, mono
sodium
salt, monohydrate.

The molecular formula C9H22NO7P2Na•H2O with a molecular weight of 359.24.

Ibandronate sodium is a white- to off-white powder.

It is freely soluble in water and practically insoluble in organic solvents

Ibandronate sodium has the following structural formula:
Determination of Ibandronate
International Journal of Pharma Sciences Vol. 4, No. 1 (2014): 442-446
Conclusion:

Statistical analysis proves that the method is repeatable, selective and accurate for the determination of investigated drug.
Full transcript