Literature survey

1. METHOD DEVELOPMENT AND VALIDATION
FOR ESTIMATION OF SOME DRUGS IN
BULK AND FORMULATION BY UV–
SPECTROPHOTOMETER AND HPLC
Submitted by
Gaikwad Abhijeet Bhimrao
M.Pharm., II Sem.
Seat no . MNB200001
Project Guide
Dr. Rana Zainuddin
M. Pharm. Ph. D.
Maulana Azad Education Trust's
Y.B.CHAVAN COLLEGE OF PHARMACY
Dr. Rafiq Zakaria Campus,
Aurangabad- 431001
Year 2017-18 1

2.  Introduction
 Need of study
 Objective
 Plan of work
 Literature survey
 Feasibility of research work
 Conclusion
 References
2

3.  Analytical method development and its significance
 Analytical method validation
 Importance of validation
 Parameters for method validation
 Specificity
 Detection limit (LOD)
 Quantification limit (LOQ)
 Linearity
 Range
 Accuracy
 Precision
 Robustness
 INSTRUMENTS USED IN ANALYTICAL METHOD DEVELOPMENT (4,5)
 UV VISIBLE SPECTROSCOPY
 HPLC
3

4.  It is essential to employ well-characterized and fully validated
analytical methods to yield reliable results that can be
satisfactorily interpreted.
 It is recognized that analytical methods and techniques are
constantly undergoing changes and improvements, and in
many instances, they are at the cutting edge of the technology.
 It is also important to emphasize that each analytical technique
has its own characteristics, which will vary from analyte to
analyte. In these instances, specific validation criteria may
need to be developed for each analyte.
4

5.  To develop and validate highly specific, reliable and cost
effective method for analysis of new drugs by using
HPLC.
 To identify and quantification of analyte.
5

6.  Literature survey
 Selection of analytical technique
 Method Development
 Method Validation
 Compilation of data
 Result & conclusion
6

7. 7
 Shahnaz Gauhar, Syed Ayub Ali, Harris Shoaib (2009) (06)
 Amar J. Chaudhari, Stuti A. Patel, Zarana N. Patel, and Dhwani T. Patel
(2011) (07)
 Ankit D. Patel, Shalin K. Parikh (2011) (08)
 V. S. Mastiholimath, P. P. Gupte1, P. M. Dandagi, A. P. Gadad (2012) (09)
 Md. Ahasan Ullah Nayon1, Jeb-Un Nesa, Md. Nasir Uddin, Md. Shah
Amran, Umme Bushra (2013) (10)
 Y.NIRUPA RANI, B.V.V RAVI KUMAR, SMITAPADMA MOHANTY
(2013) (11)
 S. A. Pagar, D.M.Shinkar, R.B.Saudagar (2013) (12)
 D Noel Preetham, K Sujana, P D S Sankar (2014) (13)
 Magda M. Ibrahim (2015) (14)
 Yuvraj Dilip Dange, Sandip Mohan Honmane, Somnath Devidas Bhinge,
Vijay Rajaram Salunkhe, Dhanraj Raghunath Jadge (2017) (15)

8. Authors and Year Research work
Shahnaz Gauhar, Syed
Ayub Ali, Harris Shoaib
(2009)
Topic: Development and Validation of a HPLC Method for Determination
of Pefloxacin in Tablet and Human Plasma
Details:
Hplc :Shim-pack CLC-ODS column
Mobile phase Acetonitrile: Phosphoric acid
Flow rate = 1 ml/min
Analysis using (UV) detector at a wavelength of 275 nm
The method is linear, quantitative, reproducible and could be used as a
more convenient, efficient and economical method for the trace analysis of
drug in biological fluids, in raw material and tablets.
Amar J.
Chaudhari, Stuti A.
Patel, Zarana N.
Patel, and Dhwani T.
Patel (2011)
Topic: To develop and validate the uv-spectrophotometric method for the
estimation of terbinafine hydrochloride in bulk and pharmaceutical
formulations as per ICH guidelines.
Details:
Absorbance maximum at 283 nm
Solvent: Distilled water
Validation: Accuracy, Precision, Sensitivity, Repeatability and Ruggedness
8

9. Authors and Year Research work
Ankit D. Patel, Shalin
K. Parikh (2011)
Topic: Development and validation of high performance liquid
chromatographic and UV spectrophotometric method for estimation of
pemetrexed disodium in bulk drug and pharmaceutical formulation
Details:
Validation parameters linearity, precision, accuracy, robustness, limit of
detection and limit of quantitation
Reversed-phase technique
Solvent: water
Absorption maximum of 225 nm
V. S. Mastiholimath, P.
P. Gupte1, P. M.
Dandagi, A. P. Gadad
(2012)
Topic: A simple and reliable UV spectrophotometric and high-performance
liquid chromatography (HPLC) methods were developed and validated for
Moexipril hydrochloride in pure form and pharmaceutical dosage form.
Details:
RP-HPLC : Agilant eclipse C 18
Mobile phase : methanol: acetonitrile (70:30% v/v)
UV spectrophotometric method was developed in phosphate buffer pH 6.8.
Calibration curve was linear.
Validation parameter:
Regression coefficient, Precision, Limits of detection and quantification
(LOQ).
9

10. Authors and Year Research work
Md. Ahasan Ullah
Nayon, Jeb-Un Nesa,
Md. Nasir Uddin, Md.
Shah Amran, Umme
Bushra (2013)
Topic: UV-Visible spectrophotometric method for the estimation of
cefixime trihydrate in bulk and pharmaceutical formulation.
Details:
Solvent: mixture of methanol and water
Absorption maximum (λmax) 287 nm.
Validation parameter
Precision, limit of detection and limit of quantification, robustness and
ruggedness
Method was precise, accurate and cost effective.
Applicable for quantitative determination of the bulk drug as well as
dosage formulation.
Y.NIRUPA RANI, B.V.V
RAVI KUMAR,
SMITAPADMA
MOHANTY (2013)
Topic: To develop and validate simple, sensitive and specific
spectrophotometric method for the determination of Carvedilol, an alpha
adrenergic receptor blocker, anti hypertensive drug in pure form and in
pharmaceutical formulations by UV visible spectroscopic methods.
Details:
Validated with respect to linearity, accuracy, precision and specificity.
Solubility and maximum sensitivity Chloroform.
The λmax or the absorption maxima of the drug was found to be 286 nm.
The calibration range was studied from 50% ‐150% and correlation was
found to be R = 0.998 10

11. Authors and Year Research work
S. A. Pagar,
D.M.Shinkar,
R.B.Saudagar (2013)
Topic: A simple, sensitive and highly accurate ultraviolet spectrophotometric
method has been developed and validated for determination of metoprolol
succinate in bulk and pharmaceutical formulations.
Details:
Solution in distilled water and phosphate buffer pH 6.8 at 221 nm and
223nm respectively in the wavelength range of 200 - 400 nm.
Beer’s law was obeyed in the concentration range of 5-25 µg/ml.
Validated in terms of
accuracy, precision, linearity, limit of detection, limit of quantification
D Noel Preetham, K
Sujana, P D S Sankar
(2014)
Topic: To develop simple, economical, precise and less time consuming UV
method for the estimation of Lisinopril in bulk and pharmaceutical
formulations.
Details:
Maximum absorbance at 218nm in absorption maxima method.
Validated in terms of
Linearity, accuracy as per the International Conference on Harmonization
(ICH) guidelines. The proposed method is recommended for routine analysis
since it is rapid, simple, accurate and sensitive.
11

12. Authors and Year Research work
Magda M. Ibrahim
(2015)
Topic: Co-administration of antihypertensive and anti-diabetic
drugs
Details:
RP-HPLC chromatographic method was developed for the
simultaneous determination of the antihypertensive drug
carvedilol (CRV) and the hypoglycemic agent glimepiride (GMP)
or glibenclamide (GBD).
Isocratic reversed phase high performance liquid
chromatographic method using a C18 column with ultraviolet
detection at 220 nm
Flow rate :1 mL/ min
mobile phase consisting of 70:30 v/v methanol: 0.2M
phosphate buffer (pH 3.5)
column temperature 30oC
binary combination laboratory prepared tablets with assay
percent range 99.49- 99.95 % and relative standard deviation
less than 1% indicating satisfactory accuracy of the method.
The method was validated according to the ICH guidelines.
12

13. Authors and Year Research work
Yuvraj Dilip Dange,
Sandip Mohan
Honmane, Somnath
Devidas Bhinge, Vijay
Rajaram Salunkhe,
Dhanraj Raghunath
Jadge (2017)
Topic: Development and Validation of UV-Spectrophotometric Method for
Estimation of Metformin in Bulk and Tablet Dosage Form
Details:
Solubility :freely soluble in water
Methodology:
Choices of a common solvent were essential so various solvent
ranges including methanol, ethanol, acetonitrile and
phosphate buffer and various concentrations ranges of various
buffers were analyzed.
Conclusion: Water was selected as a solvent for the proposed
method.
Maximum absorbance at 234 nm.
The percentage recoveries for Metformin Hydrochloride were
found in the range of 99- 101 %.
Validated in terms of
linearity, accuracy, precision, ruggedness, robustness and
recovery. The method was simple, convenient and suitable for
the determination of Metformin Hydrochloride from bulk and
tablet dosage forms.
13

14. Instrument Specification
HPLC Y.B.CHAVAN COLLEGE OF PHARMACY
1. MAKE : SHIMADZU
SOFTWARE : UV PROBE
2. MAKE : AGILENT
SOFTWARE : CHEMSTAT
3. MAKE : JASCO
SOFTWARE : CHROMNAV 2.0
UV SPECTROPHOTOMETER
Y.B. CHAVAN COLLEGE OF PHARMACY
1.MAKE : SHIMADZU
MODEL : 1800
2. MAKE : JASCO
MODEL : 630V
14

15. The project deals with development of analytical method
for analysis of some drugs which is required to assess the
quality of drug product and hence necessary for the
therapeutic effectiveness of drug.
15

16. 1. Yan Li, Gerald J Terfloth, Alireza S Kord, A systematic approach to RP-HPLC method development.
2. Shethi PD. Quantitative Analysis of Pharmaceutical Formulations, 1st Edition 2001, 11.
3. www.ICH.org Q2A “Harmonized Tripartite Guideline: Text on validation of analytical procedures”;
Proceedings of the International Conference on Harmonization, March 1994.
4. Skoog DR, Hollar FJ, Nieman TA, “Principles of instrumental analysis” 5th edition, Thomson
Brooks/Cole,2005, 300, 726.
5. Chatwal GR and Anand SK “Instrumental method of chemical analysis” 5th edition, Himalaya
Publishing House, 2007, 149-150.
6. Iranian Journal of Basic Medical Sciences Vol. 12, No. 1, Spring 2009, 33-42 Received: Nov 25
2008; Accepted: Jan 20, 2009
7. Pharm Methods. 2011 Jul-Sep; 2(3): 198–202.
8. International Journal of Drug Development & Research | April-June 2011 | Vol. 3 | Issue 2
9. The Malaysian Journal of Analytical Sciences, Vol 16 No 3 (2012): 202 – 212
10. Asian Journal of Biomedical and Pharmaceutical sciences ,2013
11. Asian Journal of Pharmaceutical and Clinical Research Vol 6, Suppl 2, 2013
12. IJPBS |Volume 3| Issue 4 |OCT-DEC|2013|224-228
13. Int. J. Pharm. Sci. Rev. Res., 25(1), Mar – Apr 2014; Article No. 43, Pages: 257-259
14. Indo American Journal of Pharmaceutical Research, Volume 5, 2015
15. Indian Journal of Pharmaceutical Education and Research | Vol 51 | Issue 4S | Oct-Dec (Suppl), 2017
16

17. Thank You
17