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VALIDATION OF ANALYTICAL PROCEDURES: A COMPARISON OF ICH Vs PHARMACOPOEIA Vs FDA


8. COMPARISON
8.1 According to USP
The performance characteristics required can be referred to as “Eight steps of  Method Validation”.  These analytical performance characteristics are
1.    Accuracy
2.    Precision
3.    Specificity
4.    Detection limit
5.    Quantiation limit
6.    Linearity and range
7.    Ruggedness
8.    Robustness

8.2 According to ICH
1.    Accuracy
2.    Precision
3.    Repeatability
4.    Intermediate precision
5.    Specificity
6.    Detection limit
7.    Quantiation limit
8.    Linearity
9.    Range
10.   Robustness
11.   System suitability

8.3 According to FDA Reviewer Guidance
1.    Accuracy
2.    Precision
3.    Repeatability
4.    Injection repeatability
5.    Analysis repeatibility
6.    Intermediate precision
7.    Specificity / selectivity
8.    Reproducibility
9.    Detection and quantiation limit
10.    Quantiation limit
11.    Linearity
12.    Range
13.    Robustness
14.    System suitability specifications and tests
15.    Sample solution stability 2

8.4 According to European guidelines
1.    Accuracy
2.    Precision
3.    Repeatability
4.    Intermediate precision
5.    Specificity
6.    Detection limit
7.    Quantiation limit
8.    Linearity
9.    Range 3

Table III -  USP data elements required for Validation13

Analytical performance parameters

Assay category I

Assay category II

Quantitative       Limit tests

Assay category   III

Assay category    IV

Accuracy

Yes

Yes

*

*

No

Precision

Yes

Yes

No

Yes

No

Specificity

Yes

Yes

Yes

*

Yes

DL

No

No

Yes

*

No

QL

No

Yes

No

*

No

Linearity

Yes

Yes

No

*

No

Range

Yes

Yes

*

*

No

* indicates may be required on nature of specific test



Table IV - ICH elements required for Validation 2

Analytical performance parameters

identification

Impurity testing

Quantitative           Limit tests

Assay

Accuracy

No

Yes

 No

Yes

Precision

 

Repeatability

No

Yes

No

Yes

Intermediate precision

No

Yes

No

Yes

Specificity

Yes

Yes

Yes

Yes

LOD

No

Yes

Yes

No

LOQ

No

Yes

No

No

Linearity

Yes

Yes

No

Yes

Range

Yes

Yes

No

Yes

 

 Table V Japanese Pharmacopoeia elements required for Validation14

Validation characteristics/ type  Of test

Identification

Impurity testing

Quantitative         Limit tests

Assay

Accuracy

No

Yes

 No

Yes

Precision

 

Repeatability

No

Yes

No

Yes

Intermediate precision

No

No*

No

No*

Reproducibility

No

No*

No

Yes*

Specificity

Yes

Yes

Yes

Yes

LOD

No

No

Yes

No

LOQ

No

Yes

No

No

Linearity

No

Yes

No

Yes

Range

No

Yes

No

Yes

* either intermediate precision or reproducibility should be evaluated depending upon circumstances in which analytical tests are performed

Table VI - Comparison of Analytical Parameters required for Validation 2

USP General chapter <1225>

ICH Q2A Guidelines

FDA Reviewer Guidance

Accuracy

Accuracy

Accuracy

Precision

Precision

 Precision

      No

      Repeatability

      Repeatability

      Injection analysis

      No

      Intermediate precision

      Intermediate precision

      No

      No

      Reproducibility

Specificity

Specificity

Specificity/selectivity

Detection limit

Detection limit

 

Detection limit

 

Quantiation limit

Quantiation limit

Quantiation limit

Linearity

 

Linearity

 

Linearity

 

Ruggedness

No

No

Robustness

Robustness

Robustness

System suitability

(discussed separately in USP 23 general chapter <621>

System suitability

 

System suitability

Sample solution stability

 

Conclusion
This article summarizes the validation parameters that are required according to the requirements of ICH Q2R(1). The paradigm shift under cGMP in the twenty - first century that requires the bench - level scientist to have the scientific and technical Understanding, product knowledge, process knowledge, and/or risk assessment abilities to appropriately execute the quality functions of analytical method validation In this article the method validation process and the minimum requirements to be included in a regulatory method are also discussed. Also a comparison between various parameters have been made i.e. in ICH, Pharmacopoeia & FDA and a table has been drawn from those observations

REFERENCES
1.    Analytical Method Validation: Principles and Practices Available from URL http://www.pharmaquality.com/Media/.../Pgs28-31_ChapterPDF.pdf (Accessed on 06-August-2011)
2.    Carstensen T. Jens, Rhodes C.T. “Drug Stability Principles and Practices” Third edition revised and expanded 2004, Marcel Dekker inc. P.NO.- 353-360
3.    European network of official medicines control laboratories “Validation of Analytical Procedures”, june 2005 Available from URL http:// www.european-accreditation.org/.../00400OMCL%2005%2047%20 DEF3  (Accessed on 08-August-2011)
4.    Guidance for Industry Q2B Validation of Analytical Procedures : Methodology, Nov.1996 Available from URL http:// www.fda.gov/downloads/. ../Guidances/ UCM 128049.pdf (Accessed on 25-July-2011)
5.    Haider Imtiaz Syed “ Validating Standard Operating Procedure” second edition 2008 published by Informa Healthcare P.No.-448-460
6.    Huber Ludwig “Validation of Analytical methods and processes” “ Pharmaceutical process Validation” 3rd edition revised & expanded 2003 Vol. 129 .Marcel dekker inc.
7.    Huber Ludwig “Validation of Analytical Methods” A Primer, 2007   Published by Agilent Technologies Available from URL http:// www.chem.agilent .com/Library /primers/Public/5990-5140EN.pdf P.NO- 4(Accessed on 09-August-2011)
8.    International Conference on Harmonization (ICH) of Technical Requirements for the Registration of Pharmaceuticals for Human use.”Validation of Analytical Procedures: Text and Methodology.ICH Q2(R1). Geneva(Nov. 2005) (Accessed on 25-July-2011)
9.    Nash A. Robert “Validation of Analytical Procedure” “Encyclopedia of Pharmaceutical Technology” 3rd edition, 2003 volume 1, edited by James Swarbrick Informa healthcare Inc. P.NO – 3928-3929
10.    Sarrio V. Robert, Silvestri J. Loui “ Validation of Analytical Assays and test methods for the pharmaceutical Laboratory”,1996 Available from URL http://www.regulatory.com/forum/article/test-val.html(Accessed on 26-July-2011)
11.    Sharma P.P “Validation in Pharmaceutical Industry- Concept, Approaches & Guidelines, First Edition 2007 Published by Vandana Publications Pvt. Ltd. P.NO 361-362
12.    Sharma P.P. “How to Practice GLP”, Second edition 2008 Published by Vandana Publications Pvt. Ltd. P.NO.-361-362
13.    U.S. Pharmacopoeia (USP) 2007 General Chapter <1225> “Validation of Compendial Procedures”, USP, Rockville, MD P.NO..-2748-2749
14.    Validation of Analytical Procedures 1330/ General Information JP XIV Available from URL http:// lib.njutcm.edu.cn/yaodian /jp/14data/ Validation_ of_Analytical  _Pr.pdf (Accessed on 10-August-2011)
15.    Validation of Analytical Procedures: Definition and Terminology, October 1998 (at step 7 for implementation) VICH (International cooperation on harmonisation of technical requirements for registration of veterinary medicinal plants) P.NO – 3 Available from URL http:// www.fda.gov/ downloads/ Animal Veterinary/ .. ./UCM052377.pdf (Accessed on 09-August-2011)
16.    WHO Expert committee on specifications for pharmaceutical preparations, thirty    second report world health organization geneva 1992  Available from URL http:// www.who.int/prequal/info_general/.../ WHO_TRS_929 _a nnex5FDCs.pdf P.NO. 4 (Accessed on 06-August-2011)

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Anonymous (not verified)
Pharma Graduate

Dear All,

With respect to the current scenario of the Indian pharma graduate and outlook of the government and the industry, we need to address the following problems with the demands as mentioned below for the pharma graduate:-

1) To ensure there are quality graduates coming out of the colleges as there are poor quality of the students coming out from the universities.

2) Our Indian degrees should be recognized all over the world and registered pharmacist in India should be able to register in any European or American Countries without much hassle.

3) As per the regulation of the price of the essential drugs in the DPCO, the salary provided to the pharma graduate should be also be regulated per the pay commission.

4) PIC (The Great Pharmacy Council of India) should work proactively for the maintaining the high standards of the pharma profession by making the employment of the pharma graduate compulsory in the production area and not allowing the other graduates including the Msc and Bsc in working in the company.

5) The DPharm graduation should be phased out immediately as there should not be any advantages or disadvantages for both the B or the D graduate.

6) The PharmD should not start as there is no scope for the further learning after Bpharm, as per the syllabus for the PharmD there is no scope for any specialization and may have no effect on any job performance. Eventually he will be standing behind a pharmacy counter which even a D pharm would be able to stand and dispense the medicine as prescribed by the doctors.

7) New Colleges having such courses should be stopped with immediate effects, as more graduates are eventually been fooled for the course and no happiness is gained by being a graduate of Pharm.

8) For Marketing Jobs, also they should be reserved only for the trained person like Dpharm or BPharm, no other untrained person should be selling the pharma products.

9) More Government Employment schemes for the further progress of the pharma profession and national strength. And allowing the Pharma graduate to have better roles in research.

For the above demands if completed, provide a perfect healthy and fairly competitive environments for the level playing of the pharma graduate. But how make the government listen to your demands, how will the bloody buggers will answer to the questions which are pertinent to their activities which are corrupt enough.

There is a solution to this question. I can make this thing happen, I require only 50 persons who can help me. The only things required:-
1) Incurring expense of rupees 50Rs (This is No payment to me)
2) Time to post an application.

If you are interested in participating in the movements, please contact me at hvk159@hotmail.com

Regards,

manav2229
Offline
Joined: 2011-11-24
GOOD WORK

I WANT TO CONGRATULATE TO ALL OF U.U ALL HAVE DONE A NICE JOB.I AM WORKING AS Sr. OFFICER VALIDATION SECTION IN MACLEODS PHARMA IN ARD FROM LAST THREE YEARS. Its A GOOD ARTICLE CAN U SEND A COPY OF THIS ON MY MAIL ID;manav2229@gmail.com. so i can read it thoroughly and give u some good suggestions.

GOOD LUCK.

Anonymous
Hi

Very Informative article. Keep it your hard work

Dr Tushar Lokhande

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